Thermally-inhibited, subsequently enzymatically hydrolysed starches and flours

0001The present invention relates to thermally-inhibited, enzymatically-treated starches and to a process for their preparation. Such starch products are useful in the preparation of food products, particularly fruit and vegetable based products.

0002Numerous starch products prepared using a variety of processes are known in the art. These include starches which are prepared by thermal inhibition or enzymatic treatment.

0003Thermally inhibited starches have been disclosed in the art. For example, European Patent Application Publication No. 0 721 471 discloses thermally inhibited starches and flours and No. 0735 827 discloses their use in food products.

0004Enzymatic treatment of starches has also been disclosed in the art. U.S. Patent No. 3,644,126 discloses a method of liquefying a starch slurry using α-amylase and then malt enzymes and glucoamylase to make a highly fermentable starch conversion syrup with a DE less than 35. U.S. Patent No. 3,922,196 discloses solubilization of a granular starch to essentially dextrose using α-amylase. U.S. Patent No. 5,445,950 discloses a method of using α-amylase to prepare slightly decomposed starch granules with a DE preferably between 0.1 and 1.0 to produce a material useful as a raw material in the sugar industry.

0005EP 182 296 discloses a granular α-amylase hydrolyzed starch for use as a dusting powder. EP 231 729 discloses a gelatinized starch hydrolysate useful as a sweetener in foods which is prepared using α- and β-amylase in a two-step process. EP 704 169 discloses partially gelatinized starch which is hydrolyzed to a DE of preferably between 4 and 10 for use as a fat or oil substitute.

0006The use of glucose syrups in a variety of foods, including ketchup, jams, marmalades and fruit preparations, has been reported in Food Review, 19(6):33 (1993). Glucose syrups are purified, concentrated aqueous <i>solutions</i> of nutritive saccharides of DE 20 or more obtained by hydrolysis of edible starch. See Whistler et al., <u>Starch Chemistry and Technology</u>, 2^nd Ed., Academic Press, Inc. Orlando, pp. 612 (1984). Further, glucose syrups known in the art do not add viscosity to food products. They are primarily added to provide or balance sweetness, as a bulking agent or filler, and to enhance Maillard browning.

0007Surprisingly, it has now been discovered that thermal inhibition followed by enzyme hydrolysis produces unique starches useful in food products, particularly vegetable- or fruit-based products.

0008The present invention is directed to a thermally inhibited, subsequently enzymatically hydrolyzed, ungelatinized, granular starch or flour and the process of making such starch or flour. Such starch or flour is useful as an ingredient in food products, particularly fruit- or vegetable-based products.

0009An object of the present invention is to provide a thermally inhibited, subsequently enzymatically hydrolyzed, ungelatinized, granular starch or flour.

0010Another object of the present invention is to provide a method of preparing a thermally inhibited, subsequently enzymatically hydrolyzed, ungelatinized, granular starch or flour.

0011Still another object of the present invention is to provide a food product containing a thermally inhibited, subsequently enzymatically hydrolyzed, ungelatinized, granular starch or flour, particularly a fruit- or vegetable-based food product.

0012A further object of the present invention is to provide a tomato-based product in which a portion of the tomato solids have been replaced by a thermally inhibited, subsequently enzymatically hydrolyzed, ungelatinized, granular starch or flour.

0013A still further object of the present invention is to provide a fruit-based product in which at least a portion of the pectin has been replaced by a thermally inhibited, subsequently enzymatically hydrolyzed, ungelatinized, granular starch or flour.

0014These and other objects of the present invention will become apparent to one skilled in the art from the following detailed description and examples below.

0015The present invention is directed to a thermally inhibited, subsequently enzymatically hydrolyzed, ungelatinized, granular starch or flour and the process of making such starch or flour. Such starch or flour is useful as an ingredient in food products, particularly fruit- or vegetable-based products.

0016All starches and flours are suitable for use herein and may be derived front any native source. A native starch or flour, as used herein, is one as it is found in nature. Typical sources for the starches and flours are cereals, tubers, roots, legumes and fruits. The native source can be corn, pea, potato, sweet potato banana, barley, wheat, rice sago, amaranth, tapioca, arrowroot, canna, sorghum, and wary or high amylose varieties thereof. As used herein, the term "waxy" is intended to include a starch or flour containing at least about 95% by weight amylopectin and the term "high amylose" is intended to include a starch or flour containing at least about 45% by weight amylose. In particular, maize, wary maize, potato, wary potato, tapioca, wary tapioca, and waxy barley, more particularly waxy maize, are useful in the instant invention.

0017Thermal inhibition is known in the art and has been disclosed, for example, in European Patent Application Publication No. 0 721 471. Native granular starches have a natural pH of about 5.0 to 6.5. When such starches are heated to temperatures above about 125°C in the presence of water, acid hydrolysis (degradation) of the starch occurs which may impede or prevent inhibition. Therefore, the dehydration conditions need to be chosen so that degradation is avoided. Suitable conditions are dehydrating at low temperatures and the starch's natural pH or dehydrating at higher temperatures after increasing the pH of the starch to neutral or above. As used herein, the term "neutral" covers the range of pH values around pH 7 and is meant to include from about 6.5 to 7.5. At a pH above about 12, gelatinization occurs more easily so a pH of below about 12 is generally more effective in the instant invention. In particular, a pH of about 8.5 to 10.5 is effective in the instant invention. The textural and viscosity benefits of the thermal inhibition process tend to be enhanced as the pH is increased although the browning also tends to increase.

0018The pH may be adjusted by any method known in the art. For example, the ungelatinized granular starch or flour may be slurried in water or another (buffered) aqueous medium, in a ratio of 1.5 to 2.0 parts by weight of water to 1.0 part of starch or flour, and the pH may be raised by the addition of any suitable base. Buffers, such as sodium phosphate, may be used to maintain the pH if needed. Alternatively, a solution of a base may be sprayed onto the powdered starch or flour until the starch or flour attains the desired pH, or an alkaline gas such as ammonia can be infused into the starch or flour. After the pH adjustment, the slurry is then either dewatered and dried, or dried directly, typically to a moisture content of from about 2 to about 15% by weight. These drying procedures are to be distinguished from the thermal inhibition process steps in which the starch or flour is dehydrated to anhydrous or substantially anhydrous and then heat treated.

0019Suitable bases for use in the pH adjustment step include, but are not limited to, sodium hydroxide, sodium carbonate, tetrasodium pyrophosphate, ammonium orthophosphate, disodium orthophosphate, trisodium phosphate, calcium carbonate, calcium hydroxide, potassium carbonate, and potassium hydroxide, and any other bases approved for use under the applicable regulatory laws. A particularly suitable base is sodium carbonate. It may be possible to use bases not approved provided they can be washed from the starch or flour so that the final product conforms to good manufacturing practices for the desired end use.

0020A thermal dehydration is carried out by heating the starch or flour in a heating device for a time and at a temperature sufficient to reduce the moisture content to less than about 1% by weight, particularly essentially 0%. In general, the temperatures used are less than about 125°C, particularly about 100 to 120°C. The dehydrating temperature can be lower than 100°C, but a temperature of at least about 100°C will be more efficient for removing moisture.

0021Representative processes for carrying out a non-thermal dehydration include freeze drying or extracting the water from the starch or flour using a solvent, particularly a hydrophilic solvent, more particularly a hydrophilic solvent which forms an azeotropic mixture with water (e.g., ethanol).

0022The solvent dehydration step may be carried out in any suitable extraction apparatus known in the art, particularly any continuous extraction apparatus.

0023For dehydration by freeze drying, the starch or flour (at a moisture of about 4 to 5%) is placed on a tray and put into a freeze dryer. A suitable bulk tray freeze dryer is available from FTS Systems of Stone Ridge, New York under the trademark Dura-Tap. The freeze dryer is run through a programmed cycle to remove the moisture. The temperature is held constant at about 20°C and a vacuum is drawn to about 50 milliTorr (mT). The starch or flour is removed from the freeze dryer and immediately placed into a suitable heating apparatus for the heat treatment.

0024After it is dehydrated, the starch or flour is heat treated for a time and at a temperature sufficient to inhibit the starch or flour. In general, heating temperatures greater than about 100°C are used. For practical purposes, the upper limit of the heat treating temperature is about 200°C. Typical temperatures are from about 120 to 180°C, particularly from about 140 to 160°C, more particularly about 160°C. The temperature selected will depend upon the amount of inhibition desired and the rate at which it is to be achieved.

0025The time at the final heating temperature will depend upon the level of inhibition desired. When a conventional oven is used, the time ranges from about 1 to 20 hours, typically about 2 to 5 hours, usually about 3.5 to 4.5 hours. When a fluidized bed is used, the times range from about 0 minutes to 20 hours, typically about 0.5 to 3.0 hours. Longer times are required at lower temperatures to obtain more inhibited starches.

0026For most applications, the thermal dehydrating and heat treating steps will be continuous and accomplished by the application of heat to the starch or flour beginning from ambient temperature. The moisture will be driven off during the heating and the starch will become anhydrous or substantially anhydrous. Usually, at these initial levels of inhibition, the peak viscosities are higher than the peak viscosities of starches heated for longer times, although there will be greater breakdown in viscosity from the peak viscosity. With continued heat treating the peak viscosities are lower, but the viscosity breakdowns are less.

0027The process may be carried out as part of a continuous process involving the extraction of the starch from a plant material.

0028The source of the starch or flour, the initial pH, the dehydrating conditions, the heating time and temperature, and the equipment used are all interrelated variables that affect the amount of inhibition.

0029The heating steps may be performed at normal pressures, under vacuum or under pressure, and may be accomplished by conventional means known in the art particularly by the application of dry heat in dry air or in an inert gaseous environment.

0030The heat treating step can be carried out in the same apparatus in which the thermal dehydration occurs. Most conveniently the process is continuous with the thermal dehydration and heat treating occurring in the same apparatus, as when a fluidized bed is used.

0031The dehydrating and heat treating apparatus can be any industrial oven, conventional oven, microwave oven, dextrinizer, dryer, mixer or blender equipped with heating devices and other types of heaters, provided that the apparatus is fitted with a vent to the atmosphere so that moisture does not accumulate and precipitate onto the starch or flour. In particular, the apparatus is a fluidized bed, particularly one in which the apparatus is equipped with a means for removing water vapor, such as a vacuum or a blower to sweep air or the fluidizing gas from the head-space of the fluidized bed. Suitable fluidizing gases include air and nitrogen, particularly dry air. For safety reasons, a gas containing less than 12% oxygen is particularly suitable.

0032Superior inhibited starches having high viscosities with low percentage breakdown in viscosity are obtained in shorter times in the fluidized bed than can be achieved using other conventional heating ovens or dryers.

0033Optional steps can be carried out to improve the color and/or flavor. They include washing the starch or flour with water and/or removing protein and/or lipid from the starch or flour prior to the dehydrating step and/or after the heat treating step. A bleaching agent (e.g., sodium chlorite) or an alkali can be used for the protein and/or lipid removal.

0034The starches or flours may be inhibited individually or more than one may be inhibited at the same time. They may be inhibited in the presence of other materials or ingredients that would not interfere with the thermal inhibition process or alter the properties of the starch or flour product.

0035The resultant thermally inhibited granular starch is then enzymatically hydrolyzed by at least one amylase capable of digesting granular starch at significant rates, particularly α-amylase, glucoamylase, or maltogenase, using techniques known in the art. The enzyme must be capable of cleaving the alpha-D-glucosidic linkages of the starch in a granular state. The amount of enzyme is dependent upon the enzyme, i.e., type, source and activity, and base starch material used as well as the amount of hydrolysis desired. Typically, the enzyme is used in an amount of from about 0.1 to about 1.0 % by weight of the starch. For example, 0.2 to 0.6% glucoamylase (AMG-300L commercially available from Novo Nordisk) has been found to be effective in the instant invention.

0036Generally the enzyme treatment is carried out at a solids level of about 10 to about 40%, depending upon the base starch being treated. A solids level of from about 15 to 35% is particularly useful, from about 18 to 23% more particularly useful, in the instant invention.

0037The pH and temperature of the slurry should be adjusted to provide effective enzyme hydrolysis. These parameters are dependent upon the enzyme to be used and are known in the art. In general, a temperature of about 22 to about 65°C is used, particularly from about 50 to about 62°C. The temperature should be kept below the gelatinization temperature, particularly about 5°C below the gelatinization temperature of the base starch material so as to maintain the starch in the granular state. In general, the pH is adjusted to about 3.5 to about 7.5, particularly from about 4.0 to about 6.0, using techniques known in the art.

0038The enzyme reaction is continued until a dextrose equivalent of at least about 5 and up to about 60, particularly about 15 to about 35, more particularly about 20 to about 30, has been achieved, or until the desired end point (i.e., sufficient degradation to provide the desired functionality for the particular application) has been reached. The end point may be determined by a change in viscosity, by reducing sugar content, or by any other method known in the art for measuring the level of enzyme degradation of the starch molecule. In general, the enzyme reaction will take from about 0.1 to about 24 hours, particularly about 0.5 to about 4 hours. The time of the reaction is dependent upon the type of starch and enzyme used, the amount of enzyme used, and the reaction parameters of solids percent, pH, and temperature.

0039Dextrose equivalent (DE) is defined as the reducing power of the hydrolysate. Each starch molecule has one reducing end; therefore DE is inversely related to molecular weight. The DE of anhydrous D-glucose is defined as 100 and the DE of unhydrolyzed starch is virtually zero.

0040The enzyme degradation is then terminated by acid deactivation as known in the art, particularly by adjusting the pH to greater than about 9.0 at a temperature greater than about 55°C for at least 30 minutes. In the alternative, the enzyme degradation may be terminated by heat deactivation as known in the art, particularly by raising the temperature to about 85 to about 95°C and maintaining it at that temperature for at least about 10 minutes to fully deactivate the enzyme. Heat deactivation is not suitable if a granular product is desired as the heat necessary to deactivate the enzyme will generally also gelatinize the starch.

0041The resultant slurry is typically adjusted to the desired pH according to its intended end use. In general, the pH is adjusted to from about 5.0 to about 7.5, particularly from about 6.0 to about 7.0, using techniques known in the art.

0042The resultant starch (hydrolysate) may be used directly in liquid form. Alternatively, the resultant starch may be recovered in powdered form by conventional techniques known in the art, including drum drying, freeze drying, and spray drying with or without gelatinization. Gelatinization may be desirable in some applications, for example, in instant products and/or products in which the starch is not cooked out.

0043The resulting starch is characterized by a relatively high viscosity, moderate cohesiveness or gel strength, heat and shear tolerance, short texture, excellent water holding ability, neutral taste, and by its unique functionality in food products, particularly fruit or vegetable based food products. Further, the resulting starch may provide many of the attributes of a cross-linked starch.

0044The resultant starches may be used at any level desired in food products, the amount being dependent upon its desired viscosity. In general, the starch will be used in an amount of from about 0.01 to about 10%, particularly from about 0.1 to about 5% by weight of the food product.

0045The resultant starch can be used in various food products including, but not limited to, dressings, including sauces, including tomato-based sauces, white sauces, and dairy-based sauces such as cheese sauces; condiments such as ketchup, salsa, and barbecue sauce; fruit preps; jellies, jams, and marmalades; pie fillings, including fruit and cream fillings; pourable dressings and spoonable dressings, including mayonnaise; graves; lite syrups; puddings; custards; yogurts; beverages, including dairy-based beverages; gazes; soups; shortenings, including margarines; processed meats; tofu; and baby foods.

0046The resultant starches are particularly useful in vegetable-based food products, particularly when a starch is desired which has a relatively high process tolerance against heat, acid, and/or shear, has a high viscosity, is stable against gelling, has a clean flavor, and/or prevents serum separation. For example, the resultant starches are particularly useful in tomato-based products such as ketchup, barbecue sauce, tomato sauce, and salsa to reduce the amount of tomato solids without loss of viscosity or texture and to add a pulpiness that is often desired. Further, in ketchup and in barbecue and tomato sauce, use of the resultant starches reduces serum separation during storage, thus improving the overall quality of the product.

0047The starches may be used to prepare tomato paste using either hot or cold break processes. "Hot break," as used herein, is intended to describe the process of preparing tomato paste from fresh tomatoes by using heat and mechanical shear to crush and homogenize the tomatoes. "Cold break," as used herein, is intended to describe the process of preparing tomato paste from fresh tomatoes by using only mechanical force to crush fresh tomatoes at mild temperatures. Cold break tomato paste requires a higher level of tomato solids to provide similar viscosity to hot break tomato paste. However, the cold break process provides better tomato flavor and color. The present starches may be used to replace at least a portion of the tomato solids in either type of tomato paste, compensating for the loss in viscosity and controlling serum separation without the undesirable cohesiveness, gelling, or starchy taste generally provided by other starches.

0048The resultant starches are also particularly useful in fruit-based food products, particularly when a starch is desired which is relatively easy to cook out at high solids, provides a short texture, controls moisture migration, has a clean flavor, and/or provides a relatively low hot viscosity during processing. For example, the resultant starches may be used in fruit preps, jams, jellies, and fruit fillings to reduce the amount of pectin or even replace it in total without a loss in viscosity. In particular, the starches are useful in fruit-based products which have a high solids content, such as fruit preps, but are also useful in a low solid systems such as low/no sugar fruit preps. When fruit preps using the resultant starches are used in yogurts, the interface that occurs between the fruit and the white mass is significantly reduced, the stir-down and mouthfeel are improved to create a smoother yogurt, the color bleed from the fruit into the white mass is reduced, and the water capacity is improved resulting in reduced syneresis upon storage.

EXAMPLES

0049The following examples are presented to further illustrate and explain the present invention and should not be taken as limiting in any regard.

Measurement of the Net Sugar Concentration

0050The net sugar concentration in the examples, when measured using a refractometer, was determined using the following procedure.

00511.5 ml of the slurry was withdrawn using a Pasteur pipette and placed into a 1.8 ml Eppendorf tube. The tube was placed into a micro centrifuge and run at a speed of 8,000-10,000 rpm for 30-60 seconds. One drop of the clear supernatant was removed and placed on a calibrated refractometer (calibrated to zero using water). The concentration of the soluble supernatant was read.

Example 1

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Starch Preparation

0052a. thermal inhibition - A 30% solids by weight wary corn starch slurry was prepared and its pH was adjusted to 9.6 using sodium carbonate. The pH adjusted starch was filtered using a basket decanter (commercially available from Reinveld) and dried using a flash drier to a moisture of 13%. The starch was then further dried in a fluidized bed reactor to less than 1% moisture at a temperature of 130°C. The starch was then heated to 160°C and held at this temperature for 145 minutes to produce a product with a Brabender viscosity of 450. The starch was then cooled to 65°C within the reactor by supplying cooling water to the jacket and introducing cold air. The starch was then reslurried to 25% solids by weight and washed. The balance of the slurry was adjusted to 14% and the pH was adjusted to 5.2 using hydrochloric acid. The slurry was washed using a disk centrifuge (commercially available from Merco), filtered using a basket decanter, and dried to 11% moisture using a flask drier. Enzyme treatment - 1.0 kg of the thermally inhibited starch at a moisture of 10.5% was slurried in 3 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 5 g of glucoamylase (AMG 300 L commercially available from Novo Nordisk) were added. The slurry was placed in a 55°C water bath and allowed to react for five hours with constant stirring. The pH was adjusted to 9.5 using sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid. b. The slurry of Example 1a was spray dried using the following conditions: <tables id="tabl0001" num="0001"><table frame="all"><tgroup cols="2" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="78.75mm" /><colspec colnum="2" colname="col2" colwidth="78.75mm" /><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">inlet temperature</entry><entry namest="col2" nameend="col2" align="left">225°C</entry></row><row><entry namest="col1" nameend="col1" align="left">outlet temperature</entry><entry namest="col2" nameend="col2" align="left">100°C</entry></row><row><entry namest="col1" nameend="col1" align="left">% solids</entry><entry namest="col2" nameend="col2" align="left">20%</entry></row><row><entry namest="col1" nameend="col1" align="left">speed</entry><entry namest="col2" nameend="col2" align="left">30-35 rpm</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">inlet tube diameter</entry><entry namest="col2" nameend="col2" align="left">¼ inch</entry></row></tbody></tgroup></table></tables>

Example 2

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Variations on the Starch Preparation

0053<ul id="ul0001" list-style="none" compact="compact"><li>a. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 90 minutes instead of 145 minutes. 100 g of the thermally inhibited starch at a moisture content of 12.0% were slurried in 200 mL of water and the pH was adjusted to 4 with dilute hydrochloric acid. 3 g (0.30% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 55°C water bath and allowed to react with constant stirring until the net sugar concentration as measured using a refractometer reached 9.0%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid and the slurry was spray dried using the procedure of Example 1b.</li><li>b. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 100 minutes instead of 145 minutes. 18.7 kg of the thermally inhibited starch at a moisture content of 12.4% were slurried in 40 L of water and the pH was adjusted to 4.0 with dilute hydrochloric acid. 46.8 g (0.25% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 58°C water bath and allowed to react with constant stirring. After 4 hours, an additional 0.05% enzyme was added and the reaction was continued until the net sugar concentration using a refractometer reached 8.5%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using a 25% solution of hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 18.6 and a moisture content of 3.8%.</li><li>c. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 160 minutes instead of 145 minutes. 20.0 kg of the thermally inhibited starch at a moisture content of 11.7% were slurred in 40 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 80 g (0.40% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 57°C water bath and allowed to react with constant stirring until the net sugar concentration as measured using a refractometer reached 9.2%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 22.6 and a moisture content of 3.8%.</li><li>d. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 135 minutes instead of 145 minutes. 20.0 kg of the thermally inhibited starch at a moisture content of 10.2% were slurried in 40 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 60 g (0.30% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 55°C water bath and allowed to react with constant stirring until the net sugar concentration as measured using a refractometer reached 8.9%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using a 25% solution of hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 21.5 and a moisture content of 4.6%.</li><li>e. The thermal inhibition of Example 1a is repeated. After thermal inhibition, 4 kg of the thermally inhibited starch are slurried in 10 L of water and the pH is adjusted to 5.0 with dilute hydrochloric acid. 40 g of maltogenase 4000 L (commercially available from Novo Nordisk) are added. The slurry is placed in a 60°C water bath and allowed to react with continuous stirring until net sugar concentration as measured using a refractometer reaches 11.5%. The pH is adjusted to 9.0 using 4% sodium hydroxide. The slurry is maintained at this pH and temperature for 30 minutes to deactivate the enzyme. The pH is then adjusted to 6.5 using dilute hydrochloric acid and spray dried as in Example 1b. The resultant starch has a DE of 20.6 and a moisture content of 4.9%.</li><li>f. The thermal inhibition of Example 1a was repeated with the exceptions that tapioca starch was used instead of waxy corn starch and the starch was held at 160°C for 105 minutes instead of 145 minutes. 20.0 kg of the thermally inhibited starch were slurried in 40 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 80 g (0.40% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 55°C water bath and allowed to react with constant stirring until the net sugar concentration as measured using a refractometer reached 6.9%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 18.7 and a moisture content of 4.0%.</li><li>g. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 135 minutes instead of 145 minutes. 5.0k g of the thermally inhibited starch at a moisture content of 10.2% were slurried in 10 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 5 g (0.10% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 50°C water bath and allowed to react with constant stirring until the net sugar concentration as measured using a refractometer reached 2.1%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using a 25% solution of hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 5.0 and a moisture content of 4.4%.</li><li>h. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 135 minutes instead of 145 minutes. 5.0 kg of the thermally inhibited starch at a moisture content of 10.2% were slurried in 10 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 20 g (0.40% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 53°C water bath and allowed to react with constant stirring overnight. The pH was adjusted to 9.5 using 4% sodium hydroxide and the slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using a 25% solution of hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 43.0 and a moisture content of 4.3%.</li><li>i. The thermal inhibition of Example 1a was repeated with the exception that the base material used was corn starch instead of waxy corn starch and the starch was held at 160°C for 120 minutes instead of 145 minutes. 8 kg of the thermally inhibited starch were slurried in 24 kg of water and the pH was adjusted to 4.0 with dilute hydrochloric acid. 32g (0.4% w/w) of glucoamylase (G-Zyme G990SP, commercially available from Enzyme Biosystem) were added. The slurry was placed in a 55°C water bath and allowed to react with constant stirring until the net sugar concentration as measured using a refractometer reached 6.9%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using a 25% solution of hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 20.8 and a moisture content of 3.6%.</li><li>j. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 135 minutes instead of 145 minutes. 5.0 kg of the thermally inhibited starch at a moisture content of 10.2% were slurried in 10 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 20 g (0.40% w/w) of glucoamylase (AMG 300 L) were added. The slurry was placed in a 53°C water bath and allowed to react with constant stirring until the net sugar concentration indicated a DE of 24.5. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using a 25% solution of hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 24.5.</li><li>k. The thermal inhibition of Example 1a was repeated. After thermal inhibition, 4 kg of the thermally inhibited starch were slurried in 10 L of water and the pH was adjusted to 5.0 with dilute hydrochloric acid. 40 g of maltogenase 4000 L (commercially available from Novo Nordisk) were added. The slurry was placed in a 60°C water bath and allowed to react with continuous stirring until the net sugar concentration indicated a DE of 21.3. The pH was adjusted to 9.0 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for 30 minutes to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid and spray dried as in Example 1b. The resultant starch had a DE of 21.3.</li><li>l. The thermal inhibition of Example 1a was repeated with the exception that the starch was held at 160°C for 100 minutes instead of 145 minutes. 9.0 kg of the thermally inhibited starch at a moisture content of 12.6% were slurried in 18 L water and the pH was adjusted to 4.0 with dilute hydrochloric acid. 27.0 g of glucoamylase (AMG 300 L) were added. The slurry was placed in a 57°C water bath and allowed to react with constant stirring until the net sugar concentration as measured using a refractometer reached 8.4%. The pH was adjusted to 9.5 using 4% sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using a 25% solution of hydrochloric acid and the slurry was spray dried using the procedure of Example 1b. The resultant starch had a dextrose equivalent of 22.2 and a moisture content of 3.6%.</li></ul>

Example 3

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Preparation of Tomato-Based Sauce (Hot Break)

0054<tables id="tabl0002" num="0002"><table frame="all"><tgroup cols="3" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Ingredient</entry><entry namest="col2" nameend="col2" align="center">Control (wt%)</entry><entry namest="col3" nameend="col3" align="center">Experimental (wt %)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="left">44.85</entry><entry namest="col3" nameend="col3" align="left">44.85</entry></row><row><entry namest="col1" nameend="col1" align="left">Tomato Paste (hot break)</entry><entry namest="col2" nameend="col2" align="left">25.00</entry><entry namest="col3" nameend="col3" align="left">25.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Sugar</entry><entry namest="col2" nameend="col2" align="left">15.00</entry><entry namest="col3" nameend="col3" align="left">12.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Vinegar</entry><entry namest="col2" nameend="col2" align="left">12.00</entry><entry namest="col3" nameend="col3" align="left">12.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Salt</entry><entry namest="col2" nameend="col2" align="left">2.90</entry><entry namest="col3" nameend="col3" align="left">2.90</entry></row><row><entry namest="col1" nameend="col1" align="left">Onion Salt</entry><entry namest="col2" nameend="col2" align="left">0.10</entry><entry namest="col3" nameend="col3" align="left">0.10</entry></row><row><entry namest="col1" nameend="col1" align="left">Celery Salt</entry><entry namest="col2" nameend="col2" align="left">0.10</entry><entry namest="col3" nameend="col3" align="left">0.10</entry></row><row><entry namest="col1" nameend="col1" align="left">White Pepper</entry><entry namest="col2" nameend="col2" align="left">0.05</entry><entry namest="col3" nameend="col3" align="left">0.05</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Starch Sample</entry><entry namest="col2" nameend="col2" align="left">0.00</entry><entry namest="col3" nameend="col3" align="left">3.00</entry></row></tbody></tgroup></table></tables>

0055The following samples were used: <ul id="ul0002" list-style="none" compact="compact"><li><u>Sample 1</u> = Corn Syrup Solid, 24 DE (FRODEX 24, commercially available from American Maize)</li><li><u>Sample 2</u> = Starch of Example 2d</li><li><u>Sample 3</u> = Maltodextrin, 5 DE (LODEX 5, commercially available from American Maize)</li><li><u>Sample 4</u> = Starch of Example 2h</li><li><u>Sample 5</u> = Starch of Example 2f</li><li><u>Sample 6</u> = Starch of Example 2g</li><li><u>Sample 7</u> = Starch of Example 2b</li><li><u>Sample 8</u> = Starch of Example 2c</li><li><u>Sample 9</u> = Corn Syrup Solid, 42 DE (STAR DRI 42R, commercially available from Staley)</li></ul>

0056The water, tomato paste and vinegar were mixed and placed in a Koruma double jacketed steam kettle. The remaining ingredients were dry blended and added to the Koruma. The mixture was heated to 90°C and held for 5 minutes. The hot mixture was homogenized using a two stage Homogenizer at 150 Bar. The hot mixture was then stirred down in a Hobart blender using speed 2 for 1 minute and the paddle for mixing. The hot mixture was used to fill jars and refrigerated at 4°C for storage. The sauces were evaluated organoleptically and for syneresis after 37 days storage with the following results: <ul id="ul0003" list-style="none" compact="compact"><li><u>Control</u> - showed pulpiness and severe syneresis.</li><li><u>Sample 1</u> - no significant difference from control.</li><li><u>Sample 2</u> - more mouthfeel than control; no visible syneresis; thicker, shorter texture, and slightly smoother in appearance than the control. (Note: mouthfeel, as used herein, refers to a coated feeling on the tongue, heaviness, and a feeling of a film on the pallet).</li><li><u>Sample 3</u> - very thin, non-viscous; texture similar to control; definite syneresis present.</li><li><u>Sample 4</u> - slightly thicker and more viscous than control; highly pulpy texture.</li><li><u>Sample 5</u> - very thick; pulpiness similar to control; light color; no syneresis.</li><li><u>Sample 6</u> - moderately thick; very smooth and slightly long in texture; moderately pulpy.</li><li><u>Sample 7</u> - no syneresis; slightly more cohesive but less thick than Sample 2.</li><li><u>Sample 8</u> - no syneresis.</li><li><u>Sample 9</u> - slightly thicker than control; extremely pulpy; syneresis visible.</li></ul>

0057Samples 1 and 7 showed the greatest degree of pulpiness.

0058The control and Samples 3 and 9 were the only ones that exhibited syneresis.

0059The viscosity and consistency of each sample was measured using a Bostwick Consistometer and the standard methodology described in 21 CFR § 155.194(b).

0060The temperature of the sample was adjusted to 20± 1°C as was the Bostwick trough. The end-to-end level of the Bostwick was adjusted by means of the spirit level placed in the trough of the instrument. The side-to-side level was adjusted by means of the built-in spirit level. The sample was then transferred to the dry sample chamber of the Bostwick, filling the chamber slightly more than level full and avoiding air bubbles. A straight edge is passed across the top of the chamber starting from the gate end to remove excess sample. The gate is released by gradual pressure on the lever, holding the instrument down at the same time to prevent movement as the gate is released. After 30 seconds, the maximum distance of flow was read. The results are listed in Table 1 below. <tables id="tabl0003" num="0003"><table frame="all"><title>Table 1</title><tgroup cols="5" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="31.50mm" /><colspec colnum="2" colname="col2" colwidth="31.50mm" /><colspec colnum="3" colname="col3" colwidth="31.50mm" /><colspec colnum="4" colname="col4" colwidth="31.50mm" /><colspec colnum="5" colname="col5" colwidth="31.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" /><entry namest="col2" nameend="col3" align="center">Boastwick @ 20°C (cm)</entry><entry namest="col4" nameend="col5" align="left">Bostwick @ 5°C (cm)</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample</entry><entry namest="col2" nameend="col2" align="center">24 hours</entry><entry namest="col3" nameend="col3" align="center">1 Week</entry><entry namest="col4" nameend="col4" align="center">24 hours</entry><entry namest="col5" nameend="col5" align="center">1 week</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Control</entry><entry namest="col2" nameend="col2" align="char" char=".">4.5</entry><entry namest="col3" nameend="col3" align="char" char=".">3.6</entry><entry namest="col4" nameend="col4" align="char" char=".">3.6</entry><entry namest="col5" nameend="col5" align="char" char=".">3.4</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 1</entry><entry namest="col2" nameend="col2" align="char" char=".">3.9</entry><entry namest="col3" nameend="col3" align="char" char=".">4.3.</entry><entry namest="col4" nameend="col4" align="char" char=".">3.7</entry><entry namest="col5" nameend="col5" align="char" char=".">3.8</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 2</entry><entry namest="col2" nameend="col2" align="char" char=".">3.7</entry><entry namest="col3" nameend="col3" align="char" char=".">3.6</entry><entry namest="col4" nameend="col4" align="char" char=".">3.1</entry><entry namest="col5" nameend="col5" align="char" char=".">2.9</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 3</entry><entry namest="col2" nameend="col2" align="char" char=".">4.1</entry><entry namest="col3" nameend="col3" align="char" char=".">---</entry><entry namest="col4" nameend="col4" align="char" char=".">4.0</entry><entry namest="col5" nameend="col5" align="char" char=".">3.7</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 4</entry><entry namest="col2" nameend="col2" align="char" char=".">3.5</entry><entry namest="col3" nameend="col3" align="char" char=".">3.9</entry><entry namest="col4" nameend="col4" align="char" char=".">3.6</entry><entry namest="col5" nameend="col5" align="char" char=".">3.8</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 5</entry><entry namest="col2" nameend="col2" align="char" char=".">3.4</entry><entry namest="col3" nameend="col3" align="char" char=".">3.6</entry><entry namest="col4" nameend="col4" align="char" char=".">3.3</entry><entry namest="col5" nameend="col5" align="char" char=".">3.0</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 6</entry><entry namest="col2" nameend="col2" align="char" char=".">3.0</entry><entry namest="col3" nameend="col3" align="char" char=".">3.4</entry><entry namest="col4" nameend="col4" align="char" char=".">3.3</entry><entry namest="col5" nameend="col5" align="char" char=".">3.3</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 7</entry><entry namest="col2" nameend="col2" align="char" char=".">3.4</entry><entry namest="col3" nameend="col3" align="char" char=".">3.3</entry><entry namest="col4" nameend="col4" align="char" char=".">3.0</entry><entry namest="col5" nameend="col5" align="char" char=".">3.0</entry></row><row><entry namest="col1" nameend="col1" align="left">Sample 8</entry><entry namest="col2" nameend="col2" align="char" char=".">3.2</entry><entry namest="col3" nameend="col3" align="char" char=".">3.4</entry><entry namest="col4" nameend="col4" align="char" char=".">2.9</entry><entry namest="col5" nameend="col5" align="char" char=".">3.1</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Sample 9</entry><entry namest="col2" nameend="col2" align="char" char=".">---</entry><entry namest="col3" nameend="col3" align="char" char=".">---</entry><entry namest="col4" nameend="col4" align="char" char=".">---</entry><entry namest="col5" nameend="col5" align="char" char=".">---</entry></row></tbody></tgroup></table></tables>

0061As can be seen from Table I, the starches of the instant invention have a higher viscosity (lower Bostwick) than standards known in the art of comparable dextrose equivalents.

0062Serum separation of the samples, after being stored for 37 days, was measured by pouring off any serum and weighing the serum. The results are given below in Table II. <tables id="tabl0004" num="0004"><table frame="all"><title>Table II</title><tgroup cols="3" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="center">Sample</entry><entry namest="col2" nameend="col2" align="center">Weight of Serum (g)</entry><entry namest="col3" nameend="col3" align="center">% Reduction</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Control</entry><entry namest="col2" nameend="col2" align="char" char=".">1.220</entry><entry namest="col3" nameend="col3" align="left">---</entry></row><row><entry namest="col1" nameend="col1" align="left">7</entry><entry namest="col2" nameend="col2" align="char" char=".">0</entry><entry namest="col3" nameend="col3" align="left">100</entry></row><row><entry namest="col1" nameend="col1" align="left">2</entry><entry namest="col2" nameend="col2" align="char" char=".">0.088</entry><entry namest="col3" nameend="col3" align="left">92.77</entry></row><row><entry namest="col1" nameend="col1" align="left">6</entry><entry namest="col2" nameend="col2" align="char" char=".">0.131</entry><entry namest="col3" nameend="col3" align="left">89.26</entry></row><row><entry namest="col1" nameend="col1" align="left">8</entry><entry namest="col2" nameend="col2" align="char" char=".">0.192</entry><entry namest="col3" nameend="col3" align="left">84.26</entry></row><row><entry namest="col1" nameend="col1" align="left">4</entry><entry namest="col2" nameend="col2" align="char" char=".">0.230</entry><entry namest="col3" nameend="col3" align="left">81.15</entry></row><row><entry namest="col1" nameend="col1" align="left">5</entry><entry namest="col2" nameend="col2" align="char" char=".">0.338</entry><entry namest="col3" nameend="col3" align="left">72.30</entry></row><row><entry namest="col1" nameend="col1" align="left">9</entry><entry namest="col2" nameend="col2" align="char" char=".">0.360</entry><entry namest="col3" nameend="col3" align="left">70.49</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">1</entry><entry namest="col2" nameend="col2" align="char" char=".">0.454</entry><entry namest="col3" nameend="col3" align="left">62.79</entry></row></tbody></tgroup></table></tables>

Example 4

-

Preparation of Tomato-Based Sauce (Cold Break)

0063<tables id="tabl0005" num="0005"><table frame="all"><tgroup cols="4" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="39.37mm" /><colspec colnum="2" colname="col2" colwidth="39.37mm" /><colspec colnum="3" colname="col3" colwidth="39.37mm" /><colspec colnum="4" colname="col4" colwidth="39.37mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Ingredient</entry><entry namest="col2" nameend="col2" align="center">Control 1 (wt%)</entry><entry namest="col3" nameend="col3" align="center">Control 2 (wt %)</entry><entry namest="col4" nameend="col4" align="center">Expt. (wt %)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="char" char=".">39.94</entry><entry namest="col3" nameend="col3" align="char" char=".">39.94</entry><entry namest="col4" nameend="col4" align="char" char=".">39.94</entry></row><row><entry namest="col1" nameend="col1" align="left">Sugar</entry><entry namest="col2" nameend="col2" align="char" char=".">15.00</entry><entry namest="col3" nameend="col3" align="char" char=".">15.00</entry><entry namest="col4" nameend="col4" align="char" char=".">11.20</entry></row><row><entry namest="col1" nameend="col1" align="left">Hot Break Tomato</entry><entry namest="col2" nameend="col2" align="char" char=".">30.00</entry><entry namest="col3" nameend="col3" align="char" char=".">0.00</entry><entry namest="col4" nameend="col4" align="char" char=".">0.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Cold Break Tomato</entry><entry namest="col2" nameend="col2" align="char" char=".">0.00</entry><entry namest="col3" nameend="col3" align="char" char=".">30.00</entry><entry namest="col4" nameend="col4" align="char" char=".">30.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Starch</entry><entry namest="col2" nameend="col2" align="char" char=".">0.00</entry><entry namest="col3" nameend="col3" align="char" char=".">0.00</entry><entry namest="col4" nameend="col4" align="char" char=".">3.80</entry></row><row><entry namest="col1" nameend="col1" align="left">Vinegar 5%</entry><entry namest="col2" nameend="col2" align="char" char=".">12.00</entry><entry namest="col3" nameend="col3" align="left">12.00</entry><entry namest="col4" nameend="col4" align="char" char=".">12.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Salt</entry><entry namest="col2" nameend="col2" align="char" char=".">2.80</entry><entry namest="col3" nameend="col3" align="char" char=".">2.80</entry><entry namest="col4" nameend="col4" align="char" char=".">2.80</entry></row><row><entry namest="col1" nameend="col1" align="left">Potassium Sorbate</entry><entry namest="col2" nameend="col2" align="char" char=".">0.01</entry><entry namest="col3" nameend="col3" align="char" char=".">0.01</entry><entry namest="col4" nameend="col4" align="char" char=".">0.01</entry></row><row><entry namest="col1" nameend="col1" align="left">Onion Salt</entry><entry namest="col2" nameend="col2" align="char" char=".">0.10</entry><entry namest="col3" nameend="col3" align="char" char=".">0.10</entry><entry namest="col4" nameend="col4" align="char" char=".">0.10</entry></row><row><entry namest="col1" nameend="col1" align="left">Celery Salt</entry><entry namest="col2" nameend="col2" align="char" char=".">0.10</entry><entry namest="col3" nameend="col3" align="char" char=".">0.10</entry><entry namest="col4" nameend="col4" align="char" char=".">0.10</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Pepper</entry><entry namest="col2" nameend="col2" align="char" char=".">0.05</entry><entry namest="col3" nameend="col3" align="char" char=".">0.05</entry><entry namest="col4" nameend="col4" align="char" char=".">0.05</entry></row></tbody></tgroup></table></tables>

Sample Starches

0064<ul id="ul0004" list-style="none" compact="compact"><li>Expt. 1 = Starch of Example 2f</li><li>Expt. 2 = Starch of Example 2b</li></ul>

0065The water, tomato paste, and vinegar were blended in a double jacketed steam kettle. The remaining ingredients were added and the mixture was heated to 90 °C. The mixture was held at this temperature for five minutes and homogenized. Control 1 was homogenized at 200 bar and the remaining samples were "homogenized" without any pressure. The homogenized mixture was stirred down using a Hobart mixer equipped with a paddle at speed 2 for one minute. The mixture was jarred and refrigerated at 4°C.

0066After 72 hours, the samples were checked and the following results were observed: <ul id="ul0005" list-style="none" compact="compact"><li>Control 1 - thick; severe serum separation</li><li>Control 2 - very thin and liquid; slight serum separation</li><li>Expt. 1 - heavy texture; no serum separation</li><li>Expt. 2 - flowable texture; no gelling; no serum separation</li></ul>

0067Bostwick consistency was measured at various times and the results are shown in Table III. <tables id="tabl0006" num="0006"><table frame="all"><title>Table III</title><tgroup cols="4" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="39.37mm" /><colspec colnum="2" colname="col2" colwidth="39.37mm" /><colspec colnum="3" colname="col3" colwidth="39.37mm" /><colspec colnum="4" colname="col4" colwidth="39.37mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Sample</entry><entry namest="col2" nameend="col2" align="center">@72 hrs, 5°C (cm)</entry><entry namest="col3" nameend="col3" align="center">@7 days, 5°C (cm)</entry><entry namest="col4" nameend="col4" align="center">@7 days, 20°C (cm)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Control 1</entry><entry namest="col2" nameend="col2" align="char" char=".">3.0</entry><entry namest="col3" nameend="col3" align="char" char=".">4.5</entry><entry namest="col4" nameend="col4" align="char" char=".">5.0</entry></row><row><entry namest="col1" nameend="col1" align="left">Control 2</entry><entry namest="col2" nameend="col2" align="char" char=".">9.0</entry><entry namest="col3" nameend="col3" align="char" char=".">8.5</entry><entry namest="col4" nameend="col4" align="char" char=".">9.0</entry></row><row><entry namest="col1" nameend="col1" align="left">Expt. 1</entry><entry namest="col2" nameend="col2" align="char" char=".">7.0</entry><entry namest="col3" nameend="col3" align="char" char=".">6.5</entry><entry namest="col4" nameend="col4" align="char" char=".">7.5</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Expt. 2</entry><entry namest="col2" nameend="col2" align="char" char=".">5.0</entry><entry namest="col3" nameend="col3" align="char" char=".">4.5</entry><entry namest="col4" nameend="col4" align="char" char=".">5.0</entry></row></tbody></tgroup></table></tables> The present starches eliminate syneresis and provide a viscosity between that of hot and cold break controls. The viscosity of either control may be more closely matched by varying the amount of starch added.

Example 5

-

Preparation of Tomato-Based Sauce

0068<tables id="tabl0007" num="0007"><table frame="all"><tgroup cols="3" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><thead valign="top"><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Ingredient</entry><entry namest="col2" nameend="col2" align="center">Control 1 (wt%)</entry><entry namest="col3" nameend="col3" align="center">Expt. (wt. %)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="left">44.85</entry><entry namest="col3" nameend="col3" align="left">44.85</entry></row><row><entry namest="col1" nameend="col1" align="left">Sugar</entry><entry namest="col2" nameend="col2" align="left">15.00</entry><entry namest="col3" nameend="col3" align="left">13.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Hot Break Tomato</entry><entry namest="col2" nameend="col2" align="left">25.00</entry><entry namest="col3" nameend="col3" align="left">25.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Vinegar</entry><entry namest="col2" nameend="col2" align="left">12.00</entry><entry namest="col3" nameend="col3" align="left">12.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Salt</entry><entry namest="col2" nameend="col2" align="left">2.90</entry><entry namest="col3" nameend="col3" align="left">2.90</entry></row><row><entry namest="col1" nameend="col1" align="left">Onion Sait</entry><entry namest="col2" nameend="col2" align="left">0.10</entry><entry namest="col3" nameend="col3" align="left">0.10</entry></row><row><entry namest="col1" nameend="col1" align="left">Celery Salt</entry><entry namest="col2" nameend="col2" align="left">0.10</entry><entry namest="col3" nameend="col3" align="left">0.10</entry></row><row><entry namest="col1" nameend="col1" align="left">White Pepper</entry><entry namest="col2" nameend="col2" align="left">0.05</entry><entry namest="col3" nameend="col3" align="left">0.05</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Sample Starch</entry><entry namest="col2" nameend="col2" align="left">0.00</entry><entry namest="col3" nameend="col3" align="left">2.00</entry></row></tbody></tgroup></table></tables>

Sample Starches

0069<ul id="ul0006" list-style="none" compact="compact"><li>Expt. 1 = Native Sago Starch (Note: 3.00 wt.% was used of this starch and 21.00 wt% sugar)</li><li>Expt. 2 = Starch of Example 2i</li><li>Expt. 3 = Starch of Example 2d</li><li>Expt. 4 = 24 DE Corn Syrup Solids</li></ul>

0070The water, tomato paste, and vinegar were blended in a double jacketed steam kettle. The remaining ingredients were added and the mixture was heated to 90 °C. The Mixture was held at this temperature for five minutes and homogenized at 200 bar. The homogenized mixture was stirred down using a Hobart mixer equipped with a paddle at speed 2 for one minute. The mixture was jarred and refrigerated at 4°C.

0071After 72 hours, the samples were checked and the results are shown in Table IV. <tables id="tabl0008" num="0008"><table frame="all"><title>Table IV</title><tgroup cols="2" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="78.75mm" /><colspec colnum="2" colname="col2" colwidth="78.75mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="center">Sample</entry><entry namest="col2" nameend="col2" align="center">Serum (g)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Control</entry><entry namest="col2" nameend="col2" align="char" char=".">1.22</entry></row><row><entry namest="col1" nameend="col1" align="left">Expt. 1</entry><entry namest="col2" nameend="col2" align="char" char=".">0.26</entry></row><row><entry namest="col1" nameend="col1" align="left">Expt. 2</entry><entry namest="col2" nameend="col2" align="char" char=".">0.24</entry></row><row><entry namest="col1" nameend="col1" align="left">Expt. 3</entry><entry namest="col2" nameend="col2" align="char" char=".">0.45</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Expt. 4</entry><entry namest="col2" nameend="col2" align="char" char=".">0.454</entry></row></tbody></tgroup></table></tables> The present starches significantly reduce syneresis and provide a viscosity between that of hot and cold break controls. The viscosity of either control may be more closely matched by varying the amount of starch added.

Example 6

-

Preparation of Tomato Sauce

0072a. <tables id="tabl0009" num="0009"><table frame="all"><tgroup cols="2" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="78.75mm" /><colspec colnum="2" colname="col2" colwidth="78.75mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Ingredient</entry><entry namest="col2" nameend="col2" align="center">Control 1 (wt%)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="left">63.52</entry></row><row><entry namest="col1" nameend="col1" align="left">Tomato Paste</entry><entry namest="col2" nameend="col2" align="left">30.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Olive Oil</entry><entry namest="col2" nameend="col2" align="left">2.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Salt</entry><entry namest="col2" nameend="col2" align="left">1.06</entry></row><row><entry namest="col1" nameend="col1" align="left">Onion Powder</entry><entry namest="col2" nameend="col2" align="left">0.19</entry></row><row><entry namest="col1" nameend="col1" align="left">Sweet Basil</entry><entry namest="col2" nameend="col2" align="left">0.09</entry></row><row><entry namest="col1" nameend="col1" align="left">White Pepper</entry><entry namest="col2" nameend="col2" align="left">0.08</entry></row><row><entry namest="col1" nameend="col1" align="left">Oregano</entry><entry namest="col2" nameend="col2" align="left">0.04</entry></row><row><entry namest="col1" nameend="col1" align="left">Garlic Powder</entry><entry namest="col2" nameend="col2" align="left">0.02</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">10 DE maltodextrin</entry><entry namest="col2" nameend="col2" align="left">3.00</entry></row></tbody></tgroup></table></tables> The water, tomato paste and olive oil were blended. The remaining ingredients were dry blended and added to the tomato mixture. The mixture was heated to 88°C (190°F) and held at that temperature for 10 minutes. The resultant tomato sauce was hot filled into jars and refrigerated at 4°C overnight. The sauce was then heated to 74°C (165°F) and Bostwick viscosity was measured for each sample at 15, 30, 45 and 60 seconds using the procedure previously described. The average of three readings are listed in Table V below. b. Example 6a was repeated except the mixture was heated to 90.6°C (195°F) instead of to 88°C (190°F) with no subsequent holds. The following formulations were used with the amount of each ingredient is listed as a weight percent. <tables id="tabl0010" num="0010"><table frame="all"><tgroup cols="3" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Ingredient</entry><entry namest="col2" nameend="col2" align="center">Control 2</entry><entry namest="col3" nameend="col3" align="left">Expt</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="left">65.02</entry><entry namest="col3" nameend="col3" align="left">63.52</entry></row><row><entry namest="col1" nameend="col1" align="left">Tomato Paste</entry><entry namest="col2" nameend="col2" align="left">30.00</entry><entry namest="col3" nameend="col3" align="left">30.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Olive Oil</entry><entry namest="col2" nameend="col2" align="left">2.00</entry><entry namest="col3" nameend="col3" align="left">2.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Salt</entry><entry namest="col2" nameend="col2" align="left">1.06</entry><entry namest="col3" nameend="col3" align="left">1.06</entry></row><row><entry namest="col1" nameend="col1" align="left">Onion Powder</entry><entry namest="col2" nameend="col2" align="left">0.19</entry><entry namest="col3" nameend="col3" align="left">0.19</entry></row><row><entry namest="col1" nameend="col1" align="left">Sweet Basil</entry><entry namest="col2" nameend="col2" align="left">0.09</entry><entry namest="col3" nameend="col3" align="left">0.09</entry></row><row><entry namest="col1" nameend="col1" align="left">White Pepper</entry><entry namest="col2" nameend="col2" align="left">0.08</entry><entry namest="col3" nameend="col3" align="left">0.08</entry></row><row><entry namest="col1" nameend="col1" align="left">Oregano</entry><entry namest="col2" nameend="col2" align="left">0.04</entry><entry namest="col3" nameend="col3" align="left">0.04</entry></row><row><entry namest="col1" nameend="col1" align="left">Garlic Powder</entry><entry namest="col2" nameend="col2" align="left">0.02</entry><entry namest="col3" nameend="col3" align="left">0.02</entry></row><row><entry namest="col1" nameend="col1" align="left">10 DE Maltodextrin</entry><entry namest="col2" nameend="col2" align="left">1.50</entry><entry namest="col3" nameend="col3" align="left">0.00</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Starch of Ex. 2d</entry><entry namest="col2" nameend="col2" align="left">0.00</entry><entry namest="col3" nameend="col3" align="left">3.00</entry></row></tbody></tgroup></table></tables> Bostwick viscosity was measured for each sample at 15, 30, 45 and 60 seconds. The average of three readings are listed in Table V below. <tables id="tabl0011" num="0011"><table frame="all"><title>Table V</title><tgroup cols="4" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="39.37mm" /><colspec colnum="2" colname="col2" colwidth="39.37mm" /><colspec colnum="3" colname="col3" colwidth="39.37mm" /><colspec colnum="4" colname="col4" colwidth="39.37mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="center">Time(s)</entry><entry namest="col2" nameend="col2" align="center">Control 1</entry><entry namest="col3" nameend="col3" align="center">Control 2</entry><entry namest="col4" nameend="col4" align="center">Expt.</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="right">15</entry><entry namest="col2" nameend="col2" align="char" char=".">11.25</entry><entry namest="col3" nameend="col3" align="char" char=".">12.5</entry><entry namest="col4" nameend="col4" align="char" char=".">7.25</entry></row><row><entry namest="col1" nameend="col1" align="right">30</entry><entry namest="col2" nameend="col2" align="char" char=".">11.33</entry><entry namest="col3" nameend="col3" align="char" char=".">12.75</entry><entry namest="col4" nameend="col4" align="char" char=".">8.12</entry></row><row><entry namest="col1" nameend="col1" align="right">45</entry><entry namest="col2" nameend="col2" align="char" char=".">11.33</entry><entry namest="col3" nameend="col3" align="char" char=".">13.00</entry><entry namest="col4" nameend="col4" align="char" char=".">8.50</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="right">60</entry><entry namest="col2" nameend="col2" align="char" char=".">11.33</entry><entry namest="col3" nameend="col3" align="char" char=".">13.25</entry><entry namest="col4" nameend="col4" align="char" char=".">8.75</entry></row></tbody></tgroup></table></tables>

Example 7

-

Preparation of Fruit Jelly

0073<tables id="tabl0012" num="0012"><table frame="all"><tgroup cols="4" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="39.37mm" /><colspec colnum="2" colname="col2" colwidth="39.37mm" /><colspec colnum="3" colname="col3" colwidth="39.37mm" /><colspec colnum="4" colname="col4" colwidth="39.37mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Ingredients</entry><entry namest="col2" nameend="col2" align="center">Control (wt.%)</entry><entry namest="col3" nameend="col3" align="center">Expt. 1</entry><entry namest="col4" nameend="col4" align="center">Expt. 2</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Frozen Fruit</entry><entry namest="col2" nameend="col2" align="left">45.00</entry><entry namest="col3" nameend="col3" align="left">45.00</entry><entry namest="col4" nameend="col4" align="left">45.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="left">55.60</entry><entry namest="col3" nameend="col3" align="left">53.20</entry><entry namest="col4" nameend="col4" align="left">54.40</entry></row><row><entry namest="col1" nameend="col1" align="left">Sugar</entry><entry namest="col2" nameend="col2" align="left">5.00</entry><entry namest="col3" nameend="col3" align="left">5.00</entry><entry namest="col4" nameend="col4" align="left">5.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Starch of Example 2l</entry><entry namest="col2" nameend="col2" align="left">0.00</entry><entry namest="col3" nameend="col3" align="left">3.00</entry><entry namest="col4" nameend="col4" align="left">1.50</entry></row><row><entry namest="col1" nameend="col1" align="left">Pectin (AF 401)</entry><entry namest="col2" nameend="col2" align="left">0.60</entry><entry namest="col3" nameend="col3" align="left">0.00</entry><entry namest="col4" nameend="col4" align="left">0.30</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Sodium Citrate</entry><entry namest="col2" nameend="col2" align="left">0.10</entry><entry namest="col3" nameend="col3" align="left">0.10</entry><entry namest="col4" nameend="col4" align="left">0.10</entry></row></tbody></tgroup></table></tables>

0074The sugar, starch, pectin and sodium citrate were mixed. The fruit and water mixture was added. The mixture was then heated to 90°C (195°F) and held for ten minutes. The solids content was reduced to approximately 62° Brix, removing 6.30 weight percent water, and the pH was adjusted to 3.0 using citric acid. The jellies were cooled to room temperature. The jellies were then evaluated using pH, Bostwick consistency and degree Brix. The results are listed in Table VI below. <tables id="tabl0013" num="0013"><table frame="all"><title>Table VI</title><tgroup cols="5" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="31.50mm" /><colspec colnum="2" colname="col2" colwidth="31.50mm" /><colspec colnum="3" colname="col3" colwidth="31.50mm" /><colspec colnum="4" colname="col4" colwidth="31.50mm" /><colspec colnum="5" colname="col5" colwidth="31.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="center">Sample</entry><entry namest="col2" nameend="col2" align="left">pH</entry><entry namest="col3" nameend="col3" align="center">30 sec Bostwick (cm)</entry><entry namest="col4" nameend="col4" align="center">60 sec Bostwick (cm)</entry><entry namest="col5" nameend="col5" align="left">Brix</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Control</entry><entry namest="col2" nameend="col2" align="char" char=".">3.07</entry><entry namest="col3" nameend="col3" align="char" char=".">4.0</entry><entry namest="col4" nameend="col4" align="char" char=".">4.5</entry><entry namest="col5" nameend="col5" align="char" char=".">59.4</entry></row><row><entry namest="col1" nameend="col1" align="left">Expt. 1</entry><entry namest="col2" nameend="col2" align="char" char=".">3.03</entry><entry namest="col3" nameend="col3" align="char" char=".">4.5</entry><entry namest="col4" nameend="col4" align="char" char=".">5.0</entry><entry namest="col5" nameend="col5" align="char" char=".">61.4</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Expt. 2</entry><entry namest="col2" nameend="col2" align="char" char=".">3.04</entry><entry namest="col3" nameend="col3" align="char" char=".">4.5</entry><entry namest="col4" nameend="col4" align="char" char=".">5.0</entry><entry namest="col5" nameend="col5" align="char" char=".">62.8</entry></row></tbody></tgroup></table></tables>

0075As can be seen from Table VI, pectin can be either partially or fully replaced by the starches of the present invention.

0076Further, sensory evaluation showed that the jellies made with the instent starches exhibited increased gloss, no serum separation and good clarity.

Example 8

-

Preparation of Strawberry Fruit Preparation

0077<tables id="tabl0014" num="0014"><table frame="all"><tgroup cols="2" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="78.75mm" /><colspec colnum="2" colname="col2" colwidth="78.75mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Ingredients</entry><entry namest="col2" nameend="col2" align="center">Amount (wt.%)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Frozen Strawberries</entry><entry namest="col2" nameend="col2" align="left">35.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Sugar</entry><entry namest="col2" nameend="col2" align="left">53.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="left">8.40</entry></row><row><entry namest="col1" nameend="col1" align="left">Experimental Starch</entry><entry namest="col2" nameend="col2" align="left">3.30</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Pectin</entry><entry namest="col2" nameend="col2" align="left">0.30</entry></row></tbody></tgroup></table></tables>

Samples

0078<ul id="ul0007" list-style="none" compact="compact"><li>24 DE corn syrup solids</li><li>Starch of Example 2a</li></ul>

0079The fruit, sugar, pectin, and water were heated to 170°F (77°C). The pectin solution was next added and the mixture was heated to 200°F (93°C) while constantly stirring. When Brix reached about 58°, the mixture was removed from heat and sufficient citric acid solution (50%) was added to adjust the pH to 3.8. The mixture was then cooled to 160°F (71°C) and filled into jars. After 24 hours, Brix, Bostwick and pH were measured using standard procedures known in the art. The results are in Table VII below. <tables id="tabl0015" num="0015"><table frame="all"><title>Table VII</title><tgroup cols="5" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="31.50mm" /><colspec colnum="2" colname="col2" colwidth="31.50mm" /><colspec colnum="3" colname="col3" colwidth="31.50mm" /><colspec colnum="4" colname="col4" colwidth="31.50mm" /><colspec colnum="5" colname="col5" colwidth="31.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Starch</entry><entry namest="col2" nameend="col2" align="left">pH</entry><entry namest="col3" nameend="col3" align="left">Brix</entry><entry namest="col4" nameend="col4" align="center">15 sec Bostwick (cm)</entry><entry namest="col5" nameend="col5" align="center">30 sec Bostwick (cm)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">24 DE CSS</entry><entry namest="col2" nameend="col2" align="char" char=".">3.37</entry><entry namest="col3" nameend="col3" align="char" char=".">58.2</entry><entry namest="col4" nameend="col4" align="left">9</entry><entry namest="col5" nameend="col5" align="left">10½</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Starch of Ex. 2a</entry><entry namest="col2" nameend="col2" align="char" char=".">3.34</entry><entry namest="col3" nameend="col3" align="char" char=".">57.8</entry><entry namest="col4" nameend="col4" align="left">5¾</entry><entry namest="col5" nameend="col5" align="left">7</entry></row></tbody></tgroup></table></tables>

0080As can be seen from Table VII, the starch of the instant invention provides a higher viscosity (lower Bostwick) than a corn syrup solid of comparable dextrose equivalent.

Example 9

-

Comparison of Thermally-Inhibited, Enzymatically-Treated Starch and Enzymatically-Treated, Thermally-Inhibited Starch

0081a. A 30% solids by weight waxy corn starch slurry was prepared and its pH was adjusted to 9.6 using sodium carbonate. The pH adjusted starch was filtered using a basket decanter (commercially available from Reinveld) and dried using a flash drier to a moisture content of 13%. The starch was then dehydrated in a fluidized bed reactor to a moisture content of less than 1% at a temperature of 130°C The dehydrated starch was then heated to 160°C and held at this temperature for 100 minutes. The starch was then cooled to 65°C within the reactor by supplying cooling water to the jacket and introducing cold air. The thermally inhibited starch was then reslurried to 25% solids by weight and washed. The balance of the slurry was adjusted to 14% and the pH was adjusted to 5.2 using hydrochloric acid. The slurry was washed using a disk centrifuge (commercially available from Merco), filtered using a basket decanter, and dried to 11% moisture content using a flask drier. 1.0 kg of the thermally inhibited starch at a moisture content of 10.5% was slurred in 3 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 5 g of glucoamylase (AMG 300 L commercially available from Novo Nordisk) was added. The slurry was placed in a 55°C water bath and allowed to react with constant stirring until a DE of about 23 was reached. The pH was adjusted to 9.5 using sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid. The slurry was spray dried using the following conditions: <tables id="tabl0016" num="0016"><table frame="all"><tgroup cols="2" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="78.75mm" /><colspec colnum="2" colname="col2" colwidth="78.75mm" /><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">inlet temperature</entry><entry namest="col2" nameend="col2" align="left">225°C</entry></row><row><entry namest="col1" nameend="col1" align="left">outlet temperature</entry><entry namest="col2" nameend="col2" align="left">100°C</entry></row><row><entry namest="col1" nameend="col1" align="left">% solids</entry><entry namest="col2" nameend="col2" align="left">20%</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">speed</entry><entry namest="col2" nameend="col2" align="left">30-35 rpm</entry></row></tbody></tgroup></table></tables> The resultant spray dried starch was a thermally inhibited, subsequently enzyme converted starch. b. 1.0 kg of waxy corn starch was slurried in 3 L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 5 g of glucoamylase (AMG 300 L commercially available from Novo Nordisk) was added. The slurry was placed in a 55°C water bath and allowed to react with constant stirring until a DE of about 23 was reached. The pH was adjusted to 9.5 using sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid. The pH was adjusted to 9.6 using sodium carbonate. The pH adjusted, enzymatically converted starch was filtered using a basket decanter (commercially available from Reinveld) and dried using a flash drier to a moisture content of 13%. The enzyme converted starch was then further dehydrated in a fluidized bed reactor to a moisture content of less than 1% at a temperature of 130°C. The starch was then heated to 160°C and held at this temperature for 100 minutes. The starch was then cooled to 65°C within the reactor by supplying cooling water to the jacket and introducing cold air. The starch was then reslurried to 25% solids by weight and washed. The balance of the slurry was adjusted to 14% and the pH was adjusted to 5.2 using hydrochloric acid. The slurry was washed using a disk centrifuge (commercially available from Merco), filtered using a basket decanter, and dried to 11% moisture content using a flask drier. The resultant starch was an enzyme converted, subsequently thermally inhibited starch. c. 1.0 kg of waxy corn starch was slurried in 3L of water and the pH was adjusted to 4.5 with dilute hydrochloric acid. 5g of glucoamylase (AMG300L commercially available from Novo Nordisk) was added. The slurry was placed in a 55°C water bath and allowed to react with constant stirring until a DE of about 23 was reached. The pH was adjusted to 9.5 using sodium hydroxide. The slurry was maintained at this pH and temperature for half an hour to deactivate the enzyme. The pH was then adjusted to 6.5 using dilute hydrochloric acid. The pH was adjusted to 9.6 using sodium carbonate. The pH adjusted starch was filtered using a basket decanter (commercially available from Reinveld) and dehydrated using a flash drier to a moisture content of 13%. The dehydrated starch was then further dried in a fluidized bed reactor to a moisture content of less than 1% at a temperature of 130°C. The starch was then heated to 160°C and held at this temperature for 160 minutes. The starch was then cooled to 65°C within the reactor by supplying cooling water to the jacket and introducing cold air. The starch was then reslurried to 25% solids by weight and washed. The balance of the slurry was adjusted to 14% and the pH was adjusted to 5.2 using hydrochloric acid. The slurry was washed using a disk centrifuge (commercially available from Merco), filtered using a basket decanter, and dried to 11% moisture content using a flask drier. The resultant starch was an enzyme converted, subsequently thermally inhibited starch.

0082Ketchup formulations were prepared using the above starches and the following formulation: <tables id="tabl0017" num="0017"><table frame="all"><tgroup cols="2" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="78.75mm" /><colspec colnum="2" colname="col2" colwidth="78.75mm" /><thead valign="top"><row rowsep="1"><entry namest="col1" nameend="col1" align="center">Ingredient</entry><entry namest="col2" nameend="col2" align="center">Amount (g)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Ketchup</entry><entry namest="col2" nameend="col2" align="left">147</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Starch</entry><entry namest="col2" nameend="col2" align="left">3</entry></row></tbody></tgroup></table></tables> The ingredients were mixed together and heated to 195°F. The ketchups were allowed to cool to room temperature overnight.

0083Five panelists tasted the ketchups. All five agreed that the ketchup made with the starch of Example 9c had the worst color, very dark, brown; and the worst flavor, brown, caramelized, burnt, sour, and musty. Five panelists agreed the ketchup made with the starch of Example 9b was too dark and three of the five also thought it had an off-note taste, described as brown and sour. All five thought the ketchup made with the starch of Example 9a, which was thermally inhibited prior to enzyme conversion, had the best color and four thought it had the best flavor, closest to that of pure ketchup.

Example 10

-

Viscosity of Thermally-inhibited Enzyme-converted Starches

a.

Hot Paste Viscosity Measurement

0084A slurry containing 5.0% starch on a dry weight basis was prepared and heated from 50°C to 94°C at a rate of 1.5°C per minute. The slurry was then held at 94°C for 10 minutes. Hot viscosity was measured while heating the paste in an RVA Series 4 Rapid Visco Analyzer (Newport Scientific, New South Wales, Australia).

b.

Cold Paste Viscosity Measurement

0085The cooked paste from the hot paste viscosity measurement was cooled to 22°C and held for 30 minutes. Using an RFS2-BD050 rheometer (Rheometrics, Piscataway, NJ), viscosity was measured during a shear sweep from 0.1 to 100 sec^-1 at 22°C. Parallel plates of 25 mm diameter were used at a distance of 1.25% mm apart. Viscosity was compared at a shear of 10 sec^-1.

0086The hot and cold viscosity measurements are shown in Table VIII below. <tables id="tabl0018" num="0018"><table frame="all"><title>Table VIII</title><tgroup cols="3" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="center">Starch</entry><entry namest="col2" nameend="col2" align="center">Hot Peak (cps)</entry><entry namest="col3" nameend="col3" align="center">Cold Peak (cps)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">EX 2b</entry><entry namest="col2" nameend="col2" align="left">190</entry><entry namest="col3" nameend="col3" align="right">435</entry></row><row><entry namest="col1" nameend="col1" align="left">EX 2d</entry><entry namest="col2" nameend="col2" align="left">197</entry><entry namest="col3" nameend="col3" align="right">351</entry></row><row><entry namest="col1" nameend="col1" align="left">EX 2c</entry><entry namest="col2" nameend="col2" align="left">146</entry><entry namest="col3" nameend="col3" align="right">303</entry></row><row><entry namest="col1" nameend="col1" align="left">EX 2f</entry><entry namest="col2" nameend="col2" align="left">75</entry><entry namest="col3" nameend="col3" align="right">263</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">EX 2l</entry><entry namest="col2" nameend="col2" align="left">234</entry><entry namest="col3" nameend="col3" align="right">388</entry></row></tbody></tgroup></table></tables>

Example 11

- Preparation of Jam

0087<tables id="tabl0019" num="0019"><table frame="all"><tgroup cols="3" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="left">Ingredient</entry><entry namest="col2" nameend="col2" align="center">Control (wt%)</entry><entry namest="col3" nameend="col3" align="center">Experimental (wt%)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">Frozen Strawberries</entry><entry namest="col2" nameend="col2" align="left">45.00</entry><entry namest="col3" nameend="col3" align="left">45.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Pectin (AF 401)</entry><entry namest="col2" nameend="col2" align="left">0.6</entry><entry namest="col3" nameend="col3" align="left">0.0</entry></row><row><entry namest="col1" nameend="col1" align="left">Sugar</entry><entry namest="col2" nameend="col2" align="left">53.20</entry><entry namest="col3" nameend="col3" align="left">56.0</entry></row><row><entry namest="col1" nameend="col1" align="left">Water</entry><entry namest="col2" nameend="col2" align="left">5.00</entry><entry namest="col3" nameend="col3" align="left">5.00</entry></row><row><entry namest="col1" nameend="col1" align="left">Water removed</entry><entry namest="col2" nameend="col2" align="left">6.20</entry><entry namest="col3" nameend="col3" align="left">6.20</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">Starch</entry><entry namest="col2" nameend="col2" align="left">0.0</entry><entry namest="col3" nameend="col3" align="left">3.00</entry></row></tbody></tgroup></table></tables>

Samples

0088<ul id="ul0008" list-style="none" compact="compact"><li>1 = Starch of Example 2k</li><li>2 = Starch of Example 2j</li></ul>

0089The pectin, 70% of the sugar and the starch were mixed. The fruit and water were mixed separately and added to the dry ingredient mixture. The remaining sugar was added and the jam mixture was heated to 195 F (90.6°C) and held while stirring constantly. When Brix reached about 62°, the mixture was removed form heat and sufficient citric acid (50% solution) was added to adjust the pH to 3.0. The mixture was cooled to room temperature and filled into jars. The jars were stored at 4°C for 24 days.

a.

Sensory Evaluation

0090<ul id="ul0009" list-style="none" compact="compact"><li>The <b>control</b> gave a short texture, high mouthfeel, and melted quickly.</li><li><b>Sample 1</b> increased in gel strength over the 24 day storage period. The texture was very similar to the control as was the sheer and transparency. However, Sample 1 syneresed less than the control</li><li><b>Sample 2</b> had an acceptable gel structure and mouthfeel and was not cohesive. It gave more film building than the control and had the same sheen and transparency as the control Sample 2 syneresed less than the control.</li></ul>

b.

Texture Analysis

0091The texture of the jams were measured using a Texture Analyzer TAXT2 (Stable Micro Systems) A 25 mm, 20° conical probe<img file="EP0897673A2_D0001.tif" /> was used to determine the force needed to penetrate 20 mm using the following parameters: <tables id="tabl0020" num="0020"><table frame="all"><tgroup cols="2" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="78.75mm" /><colspec colnum="2" colname="col2" colwidth="78.75mm" /><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">speed to surface</entry><entry namest="col2" nameend="col2" align="left">5 mm/sec</entry></row><row><entry namest="col1" nameend="col1" align="left">initial force</entry><entry namest="col2" nameend="col2" align="left">10 g force</entry></row><row><entry namest="col1" nameend="col1" align="left">speed into sample</entry><entry namest="col2" nameend="col2" align="left">0.8 mm/sec</entry></row><row><entry namest="col1" nameend="col1" align="left">depth</entry><entry namest="col2" nameend="col2" align="left">20 mm</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">speed upwards</entry><entry namest="col2" nameend="col2" align="left">0.8 mm/sec</entry></row></tbody></tgroup></table></tables>

0092The results are listed below in Table IX. <tables id="tabl0021" num="0021"><table frame="all"><title>Table IX</title><tgroup cols="4" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="39.37mm" /><colspec colnum="2" colname="col2" colwidth="39.37mm" /><colspec colnum="3" colname="col3" colwidth="39.37mm" /><colspec colnum="4" colname="col4" colwidth="39.37mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="center">Day</entry><entry namest="col2" nameend="col2" align="center">Sample 1 Peak Force (g)</entry><entry namest="col3" nameend="col3" align="center">Sample 2 Peak Force (g)</entry><entry namest="col4" nameend="col4" align="center">Control Peak Force (g)</entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">1</entry><entry namest="col2" nameend="col2" align="char" char=".">49.028</entry><entry namest="col3" nameend="col3" align="char" char=".">34.726</entry><entry namest="col4" nameend="col4" /></row><row><entry namest="col1" nameend="col1" align="left">6</entry><entry namest="col2" nameend="col2" align="char" char=".">60.404</entry><entry namest="col3" nameend="col3" align="char" char=".">40.707</entry><entry namest="col4" nameend="col4" /></row><row><entry namest="col1" nameend="col1" align="left">8</entry><entry namest="col2" nameend="col2" align="char" char=".">61.579</entry><entry namest="col3" nameend="col3" align="char" char=".">37.022</entry><entry namest="col4" nameend="col4" /></row><row><entry namest="col1" nameend="col1" align="left">10</entry><entry namest="col2" nameend="col2" align="char" char=".">67.836</entry><entry namest="col3" nameend="col3" align="char" char=".">40.682</entry><entry namest="col4" nameend="col4" align="char" char=".">160.853</entry></row><row><entry namest="col1" nameend="col1" align="left">17</entry><entry namest="col2" nameend="col2" align="char" char=".">66.776</entry><entry namest="col3" nameend="col3" align="char" char=".">39.583</entry><entry namest="col4" nameend="col4" align="char" char=".">171.115</entry></row><row rowsep="1"><entry namest="col1" nameend="col1" align="left">24</entry><entry namest="col2" nameend="col2" align="char" char=".">63.742</entry><entry namest="col3" nameend="col3" align="char" char=".">43.437</entry><entry namest="col4" nameend="col4" /></row></tbody></tgroup></table></tables>

0093Both Samples 1 and 2 gelled, gave a cuttable texture and a shiny, transparent appearance. The thermally inhibited, enzyme converted starch samples controlled serum separation and gave a short texture. Neither sample had any off-flavors.