WO1996039877A1

WO1996039877A1 - Novel mold inhibitors and methos of making and using the same

Info

Publication number: WO1996039877A1
Application number: PCT/US1996/009783
Authority: WO
Inventors: Dale F. Kuhn
Original assignee: Tillin, Inc.
Priority date: 1995-06-07
Filing date: 1996-06-07
Publication date: 1996-12-19
Also published as: NZ311890A; AU6329896A; AU726327B2

Abstract

The invention is novel mold growth inhibiting products for various food stuffs, and a method of making and using the same. The mold growth inhibiting product is generally a mixture of various compounds, including: a first compound which is generally azodicarbonamide, a second compound which is generally lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof. In a second embodiment of the invention, a third compound is added which lowers the decomposition temperature of the azodicarbonamide. The third embodiment of the invention is a liquid mixture of the above described dry mixtures and water. All embodiments of this invention are added to the food stuff in the same or greater percentages of current day mold inhibitors, yet the resultant food stuff has no off flavor, taste or color which is normally imparted by current day mold inhibitors. Additionally, the food stuffs incorporating the mold inhibiting products of this invention have increased shelf lives as the mold inhibiting products are more effective than current day mold inhibitors. The mold inhibiting products of this invention effectively inhibit mold growth in food stuffs such as corn and wheat tortillas, cream cheese, bagels, fruit fillings, and other baked goods, dairy products and, processed fruit and meat products.

Description

NOVEL MOLD INHIBITORS AND METHODS OF MAKING AND USING THE SAME

This is a continuation-in-part application of Serial No. 08/363,716 entitled "Novel Mold Inhibitors and Methods of Making and Using the Same" filed December 23, 1994, which was a continuation-in-part application of Serial No. 08/099,939 entitled

"Mold Inhibitory Compounds for Wheat Flour Products," filed July 30, 1993, which are both incorporated herein by reference.

Field of the Invention

This invention relates to novel mold growth inhibiting products for food stuffs, i.e. food preservatives generally. More particularly, this invention relates to novel compounds for inhibiting the growth of molds over a commercially reasonable time period in various food products, while eliminating the off flavor, off color and/or odor which other known food preservatives impart.

Background of the Invention

The growth of mold is a significant problem in packaged or processed foods such as dairy products, baked goods, fruit and vegetable containing products such as fruit fillings for pies or pastries, and processed meats. The growth of mold not only significantly reduces the useful shelf life of the product, thus increasing the sellers direct costs due to stale or moldy product which can not be sold; but also requires that certain items are refrigerated during shipping and/or at the market place which causes additional indirect expenses for the end seller of the product. Various food preservatives are on the market, yet when used at concentrations which effectively increase shelf life, the prior art food preservatives impart an off flavor, odor, color and/or texture to the product which is undesirable. Consequently, a need exists for a food preservative that increases the shelf life of the product while not requiring refrigeration or causing off flavor, color, odor and/or texture.

PRIOR ART Calcium propionate and potassium sorbate are recognized mold inhibitors. For example, U.S. Patent Nos. 3,900,570 and 4,416,904 both disclose the use of calcium propionate and potassium sorbate at very low concentrations as optional mold inhibitors. For example, U.S. Patent No. 3,900,570 discloses a maximum usage of calcium propionate of 0.25 parts by weight per 100 parts of flour in the finished dough, with the preferred being about 0.06 to about 0.12. Similar concentrations are disclosed in U.S. Patent No. 4,416,904. Contrarily, the novel compound of this invention may also be used at about the same ranges but also up to 5.0 percent by total weight of ingredients used to prepare the food stuff with the optimum percentage depending on the food product and the desired shelf life.

The low concentrations of mold inhibitors used in prior art products are necessary due to the off flavor, odor, taste and/or texture that is imparted by the propionate or sorbate when concentration levels are increased. To date, no one has effectively prepared a food preservative which incorporates either a propionate or sorbate such that when used at increased levels does not impart an undesirable off flavor, odor, or texture. Refrigeration has also been used to inhibit mold growth. However, for many food items, refrigeration is not available or is impractical due to limited space and excessive cost.

Consequently, a need exists for a product which inhibits the growth of mold and thus extends the shelf life of a food stuff containing the mold inhibiting product, while not imparting an off flavor, either bitter or acidic, off odor and/or texture. It is even more desirable that increased mold inhibition without adverse side effects be accomplished without the need for refrigeration. Additionally the mold growth inhibiting product should use relatively inexpensive and available ingredients in such quantities as to be commercially economical.

Summary of the Invention The present invention provides novel compounds, and methods of making and using the same, for inhibiting the growth of molds in dairy products such as cream cheese, whipped cream, and shredded cheese; baked goods such as bagels, pound cake and pastries; fried goods such as corn and wheat tortillas; fruit containing products such as fruit fillings for pies and pastries; and processed meats.

All embodiments of the novel compound include the first compound which is either azodicarbonamide or potassium bromate, preferably azodicarbonamide.

In the first embodiment, the second compound is potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid, citric acid, lactic acid, fumaric acid or mixtures thereof. In the second embodiment, a third compound which lowers the decomposition temperature of azodicarbonamide is utilized and the second compound is lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid, or mixtures thereof.

In either the first or second embodiment, the novel mold growth inhibiting product is ultimately a dry powder mixture. The manner in which either embodiment is added to the food product is dependant on the temperature at which the food product will be processed.

In conjunction with the first embodiment, if the food products will be baked or processed at temperatures of about 212°F or above, the compound is added directly to the raw ingredients used to prepare the final product. If the processing temperature is below about 212°F, the dry mixture is initially added to water in a ratio of about 0.25 lb of mold inhibiting product to every 3 ounces of water and then heated to a temperature of about 212°F to about 475°F, preferably about 400°F, for a sufficient time, about 20 to about 30 minutes, preferably 25 minutes. The resultant product is ground to about the same fineness as the azodicarbonamide before processing, about 3 μm, and then added to the other ingredients of the food product at about 0.01 to about 20.0 percent by total weight of the raw ingredients for the food stuff.

In conjunction with the second embodiment which contains the third compound, if the food stuffs will be baked or processed at temperatures of above about 140°F, the mold growth inhibiting product is added directly to the raw ingredients of the food stuff. If the processing temperature is below this range, the dry mixture of the second embodiment is added to water in a ratio of about .25 lb mold growth inhibiting product to every 3 ounces of water and then heated to a temperature of about 140°F to about 475°F, preferably about 212°F to 365°F, for a sufficient time, about 6 to about 10 minutes, preferably about 8 minutes. The resultant product is ground to about the same fineness as the azodicarbonamide before processing, about 3 5 μm, and then added to the raw ingredients of the food stuff at about 0.5 to about 5.0 percent by total weight of raw ingredients.

The third embodiment of this invention is a liquid mixture of water and a dry mixture of azodicarbonamide as the first compound, and lactic acid, citric acid, fumaric acid, potassium sorbate, sodium

10 sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid, or mixtures thereof as the second compound. The ratio of water to dry mixture is about 4:1 to about 8:1 by weight percent.

15 The fourth embodiment of this invention is a liquid mixture of water and a dry mixture of azodicarbonamide as the first compound, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of

20 propionic acid, or mixtures thereof as the second compound, and a third compound which lowers the decomposition temperature of azodicarbonamide. The ratio of water to dry mixture is about 4:1 to about 8:1 by weight percent.

In both the third and fourth embodiments, after the water is

25 added to the dry mixture, the combination is boiled for about 15 minutes and then let cool. After cooling, additional water is added to replace the amount of liquid lost during the boiling stage. The

« liquid mold growth inhibiting product is added to the food stuff at a rate of about 0.01 to about 20.0 percent by total weight of raw

30 ingredients of the food stuff. Although not wanting to be bound by one theory, it is believed by heating the mold growth inhibiting products of this invention, either during processing or before the mold growth inhibiting product is added to the raw materials of the food stuff, enables the azodicarbonamide to eliminate the off flavor, odor and texture normally imparted by current day mold growth inhibitors such as sorbates or propionates.

Brief Description of the Drawings Figure 1 is a Summary of Mozzarella Manufacturing.

Figure 2 is a Summary of Cheddar Manufacturing.

Figure 3 is a Summary of Yeast and Mold Growth on Cheeses at 25C

(76F) .

Figure 4 is a Summary of Yeast and Mold Growth on Cheeses at 4C (40F) . Figure 5 is a Summary of Chemical Data 48 Hours Post Manufacture.

Figure 6 is a Summary of Microbial Data 48 Hours Post Manufacture. Detailed Description of the Invention As required, a detailed embodiment of the present invention is disclosed herein. It is, however, to be understood that the disclosed embodiment is merely illustrative of the invention, which may be embodied in various forms. Therefore, specific structural and functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to employ the mold inhibitory compound in the appropriate products.

In accordance with the present invention, a mold growth inhibiting product is provided for wheat or corn based bakery products, dairy products, fruit containing products such as pie or pastry fillings, and processed meats. The first embodiment of the mold growth inhibiting product is a dry powder mixture comprised of a first compound which is azodicarbonamide or potassium bromate, preferably azodicarbonamide, and a second compound which is citric acid, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof, preferably calcium propionate, sodium propionate, potassium sorbate or mixtures thereof. In reference by total weight of the mold growth inhibiting product, in the first embodiment, the first compound is present in the amount of about 0.001 to about 5.0 percent by weight, preferably about 0.001 to about 0.01; and the second compound is present in the amount of about 99.999 to about 95.0 percent by weight, preferably 99.999 to about 99.99.

Azodicarbonamide is an organic salt normally used as a dough conditioner or oxidizing agent in the food industry. It is also used as a blowing agent in the rubber industry. Azodicarbonamide is normally used in baked goods to reduce the stickiness of the dough which in turn makes processing easier. To date, it has not been used or approved as an ingredient for mold inhibiting products. In fact, FDA approval has only issued for using azodicarbonamide as a maturing or oxidizing agent. Consequently, the inventor is currently acquiring FDA approval for the use of azodicarbonamide in conjunction with mold growth inhibitors.

Azodicarbonamide is commercially available under the trademark "AZ-130", from the Sherex Chemical Company of New York as well as other sources. The other compounds are also commercially available from several different sources. If the first embodiment will be added to food stuffs which are exposed to temperatures above about 212°F during processing, the first embodiment is added directly to the raw ingredients of the food stuff at about 0.01 to about 20.0 percent by total weight of raw ingredients, preferably about 0.5 to about 5.0 percent.

If the food stuff will not be exposed to temperatures of above about 212°F, the first embodiment is added to water in a ratio of about 0.25 lb of first embodiment to every 3 ounces of water and then heated to a temperature of about 212°F to about 475°F, preferably about 400°F, for a sufficient time, about 20 to about 30 minutes, preferably 25 minutes. The resultant product is ground to about the same fineness as the azodicarbonamide before processing, about 3 μm, and then added to the raw ingredients of the food product at about 0.01 to about 20.0 percent by total weight of raw ingredients used to produce the food stuff.

The second embodiment comprises the first compound as discussed in reference to the first embodiment, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof, preferably calcium propionate, sodium propionate, potassium sorbate or mixtures thereof as the second compound, and a third compound which reduces the decomposition temperature of azodicarbonamide. The third compound is a metal oxide such as zinc oxide, a metal salt, a organometallic complex such as barium, zinc, or calcium stearate, or other compounds such as citric acid, triethanol amine, or calcium sulfate, the preferred being citric acid or zinc oxide.

In reference by weight of mold growth inhibiting product, in the second embodiment, the first compound is present in the amount of about 0.001 to about 5.0 percent by weight, preferably about 0.001 to about 0.01; the second compound is present in the amount of about 99.995 to about 70.0 percent by weight, preferably 99.995 to about 98.59; the compound is present in the amount of about 0.004 to about 30.0 percent by weight, preferably 0.004 to about 1.4.

Again, whether initial processing of the second embodiment of the mold inhibitory compound is required will be dependant on the temperature at which the food stuff is processed.

If the food stuff will be processed at temperatures above about 140°F, the second embodiment of the mold growth inhibiting product is added directly to the raw ingredients of the food stuff. If the processing temperature is below this range, the second embodiment is added to water in a ratio of about 0.25 lb of the second embodiment to every 3 ounces of water and then heated to a temperature of about 140°F to about 475°F, preferably about 212°F to about 365°F, for a sufficient time, about 6 to about 10 minutes, preferably about 8 minutes. The resultant product is ground to about the same fineness as the azodicarbonamide before processing, about 3 μm, and then added to the other raw ingredients of the food stuff at about 0.01 to about 20.0 percent, preferably about 0.5 to about 5.0 percent by total weight of the raw ingredients used to prepare the food stuff.

The third embodiment of the novel mold growth inhibiting product of this invention is comprised of about 1 part by weight of dry mixture to about 4 to 8 parts by weight of water. For example, 100 g of dry mixture would be mixed with about 400 to about 800 grams of water, preferably about 600 grams. The dry mixture is comprised of a first compound as discussed above in reference to the first embodiment, and a second compound which is citric acid, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof, preferably calcium propionate, sodium propionate, potassium sorbate or mixtures thereof.

In reference by weight of mold growth inhibiting product, in the third embodiment, the first compound is present in the amount of about 0.001 to about 5.0 percent by weight, preferably about 0.001 to about 0.01; the second compound is present in the amount of about 99.999 to about 95.0 percent by weight, preferably 99.999 to about 99.99.

The fourth embodiment of the novel mold growth inhibiting product of this invention is comprised of about 1 part by weight of dry mixture to about 4 to 8 parts by weight of water. For example, 100 g of dry mixture would be mixed with about 400 to about 800 grams of water, preferably about 600 grams. The dry mixture is comprised of a the first compound discussed above in reference to the first embodiment, a second compound which is lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid and mixtures thereof, preferably calcium propionate, sodium propionate, potassium sorbate or mixtures thereof, and a third compound which lowers the decomposition temperature of the first compound which was previously described above in relation to the second embodiment.

In reference by weight of mold growth inhibiting product, in the fourth embodiment, the first compound is present in the amount of about 0.001 to about 5.0 percent by weight, preferably about 0.001 to about 0.01; the second compound is present in the amount of about 99.995 to about 70.0 percent by weight, preferably 99.995 to about 98.59; the third compound is present in the amount of about 0.004 to about 30.0 percent by weight, preferably 0.004 to about 1.4. The third and fourth embodiments are prepared by dissolving the dry mixture in the water to form a first product. The first product is then boiled for about 15 minutes to form a second product. The second product is allowed to cool and then filtered to remove any non-liquid residue. Additional water is then added to the filtered second product to replace the liquid lost during boiling.

The third and fourth embodiments are added directly to the raw materials of the food stuff or if the food stuff is a liquid in final form, the third embodiment may be added directly to the final food stuff. The third and fourth embodiments are added at about 0.01 to about 20.0 percent by weight of raw ingredients of final food stuff, preferably 0.5 to about 5.0 percent by weight.

All embodiments can be added directly to the raw ingredients for preparing the food stuff. For example, either the first or second embodiment can be incorporated into wheat flour dough by adding it to the flour. Either one of the four embodiments could be added to the moist dough, although the addition of the third and fourth embodiment may be less desirable as it adds additional water into the dough.

As an example of how to prepare tortillas comprising the mold growth inhibiting product of this invention, when making wheat tortillas, the preferred ratio is one percent (1%) of the mold growth inhibiting product of the first or second embodiment to the weight of the dry flour mix, although effective results have been obtained with a one half percent ( %) to one and one half percent (1^%) . Satisfactory results have been obtained utilizing the following formula for the mold growth inhibiting product of the first embodiment. INGREDIENT PERCENT BY WEIGHT

Azodicarbonamide 0.004%

Potassium Sorbate 49.998%

Calcium Propionate 49.998% Table 1

These percentages are considered optimal for tortillas; however, differing percentages may be appropriate under other circumstances.

For example, certain wheat flour mixtures may require smaller or greater percentages. The percentages provided are intended to be exemplary of a preferred composition.

The following examples are set forth to exemplify the invention and should not be used to limit the invention.

Example IA In tests conducted by the American Institute of Baking, a commercially produced tortilla flour was produced using 500 grams of QUAKER flour mix and 215 grams of water at 100° F. The water and flour mixture was mixed at two minutes at a low speed and for another two minutes at a higher, second speed with a dough hook. The dough was allowed to stand for five minutes and then divided into 50-gram balls which were heat pressed at 175° F. The raw tortillas were then baked on a griddle at 450° F for 30 seconds on each side with each side heated two times.

Tests were conducted under controlled conditions with certain flour tortillas identified as control specimens. Certain other specimens were prepared using 1.0 percent by weight of the mold growth inhibiting product of this invention and 99.0 percent by weight of flour mixture in accordance with the same procedure set forth above for the control specimens. Tortillas from each test batch were evaluated after baking for flavor, odor, eating quality, and mold. The mold growth inhibiting product was comprised of the percentages set forth above in Table 1.

A first test batch of each set were heat sealed in cellophane bags, double-bagged in ziplock freezer pouches and stored at 25° C. A second test batch of each set of tortillas were inoculated with mold colonies isolated from previously molded bakery products and then also stored at 25° C.

All test batches of tortilla samples were checked daily for visual signs of mold growth over a 21-day period. By the end of the seventh day, visible signs of mold were present on the control wheat flour tortillas. However, the tortilla specimens containing the mold growth inhibiting product of this invention had not molded by the end of the 21-day test. Additionally, tortillas containing the disclosed mold inhibitory composition had no off flavor or undesirable texture at the 21-day period or at any time after baking. From the results of this test, The American Institute of Baking concluded that the disclosed mold growth inhibiting product is an effective mold inhibitor in the production of wheat flour tortillas.

Example IB

Additional tests were run using the method of preparation disclosed in Example IA. The tortillas (both the control batch and the batch containing the mold inhibitory compound) were subjected to 90° F for a period of 30 days. After such extreme conditions, the tortillas containing the mold growth inhibiting product of this invention still exhibited no mold growth, although under the extreme conditions the tortillas did have a stale taste. Example IC

Tests were also run comparing the tortillas prepared in accordance with the procedure outlined in Example IA with tortillas containing 1.5 percent of a commercially available mold inhibitor. Both sets of tortillas did not mold after 21 days. However on day 1, the tortillas containing the commercially available mold inhibitor had a very acidic taste whereas the tortillas containing the mold growth inhibiting product of this invention had no acidic taste. Taste tests were run again at the 14 day mark. The tortillas containing the commercially available mold inhibitor had a bitter taste whereas the tortillas containing the mold growth inhibiting product of this invention had no acidic taste.

Example 2A Tests were performed on corn tortillas manufactured with MASECA corn flour. One set included 0.7% by weight of sodium propionate as representative of a commercially available mold inhibitor. The other set included 1.0% of the mold growth inhibiting product of this invention as set forth in Table 1. The tortillas were prepared similarly to the method disclosed in

Example IA. During the testing period, the humidity was maintained at 90% and the temperature was maintained at 115° F.

The dough and the tortillas of the test batch that contained the sodium propionate was off color with a light yellow appearance. No off color existed in the dough or the tortillas of the test batch containing the mold inhibitor of this invention. Other characteristics such as odor, flavor, and palatability were comparable. The tortillas containing sodium propionate molded within 7 days. The tortillas containing the mold inhibitor as set forth in Table 1 molded in 13 days.

Example 2B

Tests were performed on corn tortillas manufactured with MASECA corn flour. One set included 0.7% by weight of sodium propionate as representative of a commercially available mold inhibitor. The other set included 1.0% of the mold growth inhibiting product of this invention encompassing the second embodiment. The mold inhibitor was comprised of 0.088% by weight of citric acid, 49.954% by weight calcium propionate, 49.954% by weight potassium sorbate, and .004% by weight of azodicarbonamide.

The tortillas were prepared similarly to the method disclosed in Example IA. During the testing period, the humidity was maintained at 90% and the temperature was maintained at 115° F.

The dough and the tortillas of the test batch that contained the sodium propionate was off color with a light yellow appearance. No off color existed in the dough or the tortillas of the test batch containing the mold inhibitor of this invention. Other characteristics such as odor, flavor, and palatability were comparable.

The tortillas containing sodium propionate molded within 7 days. The tortillas containing the mold inhibitor of this invention molded in 15 days.

Example 3

Tests were run to determine the effectiveness of the disclosed mold inhibitor compound in Neufchatel Cheese (cream cheese) . Each sample included 8 ounces of cream cheese. Four different test batches were prepared. The first was a control with no mold growth inhibiting products added. The remaining 3 batches contained, 0.750%, 0.500%, and 0.250%, respectively of a mold growth inhibiting product of this invention comprised of 0.088% by weight of citric acid, 49.954% by weight calcium propionate, 49.954% by weight potassium sorbate, and .004% by weight of azodicarbonamide.

Except for the control, all samples were heated to 212°F and held at that temperature for five minutes. The samples were then placed on aluminum foil. After cooling, all samples were covered with plastic wrap.

On Day 3 the control began to exhibit mold. On Day 7, the 0.250% sample began to show slight yellowing on the plastic wrap. On Day 17 the test was discontinued and the remaining samples tested. No mold appeared on either sample. Additionally the taste was good and the no offensive odor existed in either sample.

Example 4

Tests were run to determine the effectiveness of a mold growth inhibiting product of this invention in cream cheese that is applied to a pre-formed, refrigerated Danish-style pastry dough.

0.25%, 0.50% and 0.625% respectively of a mold growth inhibiting product of this invention comprised of 0.088% by weight of citric acid, 49.954% by weight calcium propionate, 49.954% by weight potassium sorbate, and .004% by weight of azodicarbonamide, was added to 8 ounces of cream cheese. The cream cheese was then applied to the center of a pre-formed, refrigerated Danish-style pastry dough. The samples were baked at 383°F-392°F, placed on aluminum foil, cooled, an_d packaged in polyethylene zipper closed bags and held at 32°C. No off-odor or off-taste was noted at the baking stage. By Day 3, noticeable mold spots were forming on the control cheeses. By Day 6, all of the control rolls were developing molds. The test was terminated after 19 days. Despite heavy mold infestation of the rolls themselves, the cream cheese which contained the mold inhibiting product did not show signs of mold.

Example 5

Two sampled of corn tortillas were prepared. The first sample (TI) was prepared by mixing 2 cups flour, 1 and ^ cup water, and 4.275 g of calcium propionate as the mold inhibiting product. The second sample (T2) was prepared by mixing 2 cups flour, 1 and *s cup water, and 4.275 g of the mold inhibiting product of this invention which was comprised of 0.004% by weight of azodicarbonamide, 0.004% by weight of citric acid and the remainder being calcium propionate. For each sample, all ingredients were mixed and 40 gram balls were flattened into approximately 6" round tortillas. The tortillas were each cooked on a hot griddle for approximately three minutes and then allowed to cool.

The pH of the dough and the finished product dissolved in water were taken. Odor and taste tests were also run with 5 being the best and 1 being the worst. The results are recorded below. The first number is the number of persons and the second number is the rating.

TEST Tl Results T2 Results pH Raw 5.60 5.77 ppHH ffiinniisshheedd 5 5..6644 5.50

Odor 6/5 6/5

Taste 6/5 6/5

Best Overall 3/1, 3/2 3/1, 3/2 From the results listed above, no difference in taste or odor was initially found and no preference was indicated by the participants of the test.

After sampling and testing was complete, the tortillas were placed in an environment chamber maintained at about 80 to 85 F and monitored daily for signs of mold. After 19 days the test was discontinued. Neither product showed signs of mold but Tl had a distinctive, unpleasant odor while T2 had no unpleasant odor.

Example 6

Five samples of apple walnut muffins were prepared using the following recipe. 127.69 g flour, 39.84 g crisco, 45.45 g sugar, 25.54 g eggs, 3.58 g eggs, 4.26 g baking powder, .72 g cinnamon, 1/10 tsp. nutmeg, 68.44 g milk, 58.26 g shredded peeled apples, and 45.97 g walnut. Tl was the control and included no mold inhibiting agent. T2 included 1.27 g of mold inhibiting product comprised of 0.004% by weight of citric acid, 0.004% azodicarbonamide, and the remainder being calcium propionate. T3 included 1.91 g of mold inhibiting product comprised of 0.004% by weight of citric acid, 0.004% azodicarbonamide, and the remainder being calcium propionate. T4 included 1.27 g of mold inhibiting product comprised of 19.0% by weight of citric acid, 0.004% azodicarbonamide, and the remainder being calcium propionate. T5 included 1.91 g of mold inhibiting product comprised of 19.0% by weight of citric acid, 0.004% azodicarbonamide, and the remainder being calcium propionate.

All five samples were baked for 18 minutes at 375F. Each were cooled and then placed in individual plastic zipper locked bags.

Tests were run on each sample, including the pH of the flour and mold inhibiting product dissolved in water, the pH of a portion of a baked muffin dissolved in water, and the odor and taste of the baked muffin. The following results were obtained with 5 being the best and 1 being the worst and the first number being the number of people issuing the rating.

Sample pH Flour pH muff. Ln Odor Taste

Tl 7.32 7.02 3/5,1/4, 1/3 2/4,1/5,2/3

T2 6.72 6.58 4/5,1/5 4/5,1/5

T3 6.53 6.28 4/5,1/4 4/5,1/4

T4 6.92 6.78 3/5,2/4 3/5,1/3,1/4

T5 7.01 6.85 5/5 3/5,1/4/,1/3

The samples were monitored daily for signs of mold. Signs of mold appeared in three days on Tl, five days in T2, six days in T3, 12 days in T4 and 9 days in T5.

Example 7

10 samples (T1-T10) of flour tortillas were prepared by adding the indicated percentage by weight of flour of a mold growth inhibiting product of this invention to 454 g of all purpose flour and mixing with 236.08 g water for each sample. The following formulations of mold growth inhibiting product and percentages were used.

Sample Percentage Formulation by Weight%

Tl 0.0 Control - no mold growth inhibitor added

T2 1.0 71% Sodium Propionate, 28.996% Citric Acid, and 0.004% Azodicarbonamide

T3 1.0 99.992% Calcium Propionate, 0.004% Citric

Acid, and 0.004% Azodicarbonamide T4 1.0 99.992% Sodium Propionate, 0.004% Zinc

Oxide, and 0.004% Azodicarbonamide T5 1 . 0 99.992% Calcium Propionate, 0.004% Zinc Oxide, and 0.004% Azodicarbonamide

T6 1. 0 64.998% Calcium Propionate, 34.998% Potassium Sorbate, and 0.004% Azodicarbonamide

T7 1 . 0 80.998% Calcium Propionate, 18.998% Citric Acid, and 0.004% Azodicarbonamide

T8 1 .0 80.998% Sodium Propionate, 18.998% Citric Acid, and 0.004% Azodicarbonamide

T9 1 . 0 80.998% Sodium Propionate, 18.998% Zinc Oxide, and 0.004% Azodicarbonamide

T10 1. 0 80.998% Calcium Propionate, 18.998% Zinc Oxide, and 0.004% Azodicarbonamide

For each sample, all ingredients were mixed and 40 gram balls were flattened into approximately 6" round tortillas. The tortillas were each cooked on a hot griddle at 450F to 475F for approximately three minutes and then allowed to cool .

All samples were placed in an environmental chamber maintained at 80F to 85F. Samples were checked daily for mold growth. The test was started on 4/21/95 and 4/24/95. The test was terminated on 5/22/95. The following results were obtained.

Sample Start Date Termination Date (When mold appeared)

Tl 4/21/95 4/26/95

T2 4/21/95 5/22/95 (still mold-free)

T3 4/21/95 5/22/95 (still mold-free)

T4 4/21/95 4/29/95

T5 4/21/95 4/30/95

T6 4/24/95 5/10/95 T7 4/24/95 5/10/95

T8 4/24/95 5/22/95 (still mold-free)

T9 _' 4/24/95 5/4/95

T10 4/24/95 5/5/95 Taste tests were also completed after the products were grilled. The following results were obtained.

Sample Taste Test Findings

Tl No odor, good taste

T2 Slight smell, good taste T3 No odor, good taste

T4 No odor, good taste

T5 No odor, good taste

T6 No odor, good taste

T7 No odor, good taste T8 No odor, good taste

T9 No odor, good taste

T10 No odor, good taste

On samples Tl through T5, the preferred sample was either Tl, T2, or T3, no one being able to differentiate one from the other. On samples T6 through T10, no one could differentiate between the samples.

Example 9

Testing was performed on prior art mold inhibitors and samples of the mold growth inhibiting products of this invention to determine pH, color, odor, and taste of the various products.

A pre-pH test was run on each sample by mixing 5 grams of sample with 45 grams of water. The pre-pH test results are listed below. For the remaining tests, each sample mixture consisted of 45 grams of mold inhibiting product and 30 grams of water. Each sample was dried in a 380F oven for 20 minutes and then allowed to dry completely in a 250F oven for up to 10 minutes longer. The color, odor and taste of each treated sample was then recorded. Post pH was also taken of the treated sample by adding 5 grams of the treated sample with 45 grams water.

The samples were comprised of the following ingredients in weight percent, Tl - 100% Potassium Sorbate; T2 - 100% Sodium Propionate; T3

- 100% Calcium Propionate; T4 - 100% Citric Acid; T5 - 99.992% Potassium Sorbate, 0.004% Citric Acid and 0.004% Azodicarbonamide; T6

- 99.992% Potassium Sorbate, 0.004% Zinc Oxide and 0.004% Azodicarbonamide; T7 - 99.992% Potassium Propionate, 0.004% Citric Acid and 0.004% Azodicarbonamide; T8 - 99.992% Potassium Propionate, 0.004% Zinc Oxide and 0.004% Azodicarbonamide; T9 - 99.992% Calcium Propionate, 0.004% Citric Acid and 0.004% Azodicarbonamide; T10 - 99.992% Calcium Propionate, 0.004% Zinc Oxide and 0.004% Azodicarbonamide; Til - 99.992% Citric Acid, 0.004% Zinc Oxide and 0.004% Azodicarbonamide; and T12 - 99.996% Citric Acid and 0.004%. Azodicarbonamide.

The following results were recorded.

# Pre-pH Post-pH Color Odor Taste

Tl 9.12 9.56 Off-White Slight Slightly Bitter

T2 7.92 9.56 Off-White Slight Slightly Bitter

T3 8.01 8.97 Off- hite - Slight Slightly Bitter

T4 1.90 1.86 Orange Slight Bitter

T5 7.41 8.68 Light Cream None None

(Lighter than control)

T6 7.41 8.89 Light Cream None None

(Lighter than control)

T7 7.19 8.76 White None None T8 7.68 8.56 White None None T9 7.48 7.28 White None None

T10 7.45 7.39 White None None

Til 1.68 1.46 Clear None Not as Tangy

T12 1.80 1.44 Clear None Not as Tangy

Example 10

Field tests were designed to determine the effectiveness of the mold growth inhibitors of this invention on all aspects of cheese manufacture, maturation, functionality and flavor. The protocol was designed with Vat 1 being the Control, i_e . no mold growth inhibitor added, Vat 2 including 0.25 percent by weight of total raw ingredients for preparing the cheese product being a mold growth inhibitor of this invention, and Vat 3 including 0.50 percent by weight of total raw ingredients for preparing the cheese product being a mold growth inhibitor of this invention. The mold growth inhibitor was comprised of 49.991% by weight calcium propionate, 49.991% by weight potassium sorbate, 0.004% by weight citric acid, and 0.004% by weight azodicarbonamide.

Figure 1 illustrates the parameters used in preparing the mozzarella cheese. Figure 2 illustrates the parameters used in preparing the cheddar cheese. The mold growth inhibitor was listed as Substance X and was added two minutes after vatting.

After manufacture, the cheese samples were cut into blocks approximately 1 kg (2.2 lb) to simplify subsequent sampling. The mozzarella blocks were stored at -2C and the cheddar blocks were stored at IOC.

At 48 hours post manufacture the chemical composition of the cheese products were evaluated. These results are shown in Figure 5. Also at 48 hours post manufacture the microbial composition of the cheese products were evaluated. These results are shown in Figure 6.

Immediately after the block samples were prepared, 2 x 100 gram samples were shredded from the block samples and placed in zip-lock bags at 25C and 4C. Each sample was examined visually each day for mold growth. The results of the 25C test are recorded in Figure 3. As shown, after 30 days, no mold was present on either the cheddar sample containing the mold growth inhibitor of this invention.

Partial results of the 4C test are shown in Figure 4. At 19 days into the 30 day test, the mozzarella sample containing 0.5% of the mold growth inhibiting product of this invention and both the cheddar samples were mold free.

Immediately after the samples were prepared, the samples containing the mold growth inhibitor of this invention were evaluated and given points for flavor, background, bitterness, etc. From a possible 105 points, the mozzarella samples containing the mold growth inhibitor of this invention were awarded 92 points giving an 88% rating. From a possible 72 points, the cheddar was awarded 67 points for a 93% rating. While this invention has been described in relation to the preferred embodiment, it is to be understood that various modifications thereof will now be apparent to one skilled in the art upon reading this specification, and it is intended to cover such modifications which fall within the scope of the following claims.

Claims

C L A I M SWhat is claimed and desired to be secured by Letters Patent is as follows:

1. A mold growth inhibiting product for food stuffs, comprising a mixture of: a) a first compound, wherein said first compound is azodicarbonamide; and b) a second compound, wherein said second compound is citric acid, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof.

2. The mold growth inhibiting product of Claim 1, wherein said second compound is potassium sorbate, calcium propionate, sodium propionate or mixtures thereof.

3. The mold growth inhibiting product of Claim 2, comprising a) about 0.001 to about 5.0 percent by total weight of said mold growth inhibiting product of said first compound; and b) about 95.0 to about 99.999 percent by total weight of said mold growth inhibiting product of said second compound.

4. The mold growth inhibiting product of Claim 1, wherein a) said second compound is lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate. nnt-ag inm propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and b) further comprising a third compound for lowering the decomposition temperature of said first compound.

5. The compound of Claim 4, wherein said third compound is a metal oxide, metal salt, organometallic complex, citric acid, calcium sulfate, triethanol amine or mixtures thereof.

6. The compound of Claim 5, wherein a) said second compound is potassium sorbate, sodium propionate, calcium propionate or mixtures thereof; and b) said third compound is citric acid, zinc oxide, or mixtures thereof.

The compound of Claim 4, comprising a) about .001 to about 5.0 percent by total weight of said mold growth inhibiting product of said first compound; b) about 65.0 to about 99.995 percent by total weight of said mold growth inhibiting product of said second compound; and c) about .004 to about 30.0 percent by total weight of said mold growth inhibiting product of said third compound.

8. A mold growth inhibiting product for food stuffs, comprising a mixture of: a) about 1 part by weight of dry mixture, wherein said dry mixture is comprised of: i) about .001 to about 5.0 percent by total weight of said dry mixture of a first compound, wherein said first compound is azodicarbonamide; and ii) about 95.0 to about 99.999 percent by total weight of said dry mixture of a second compound, wherein said second compound is acetic acid, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and b) about 4 to 8 parts by weight of water.

9. The mold growth inhibiting product of Claim 8, comprising a) about 65.0 to about 99.995 percent by total weight of said dry mixture of said second compound, wherein said second compound is lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and b) about .004 to about 30.0 percent by total weight of said dry mixture of a third compound, wherein said third compound lowers the decomposition temperature of said first compound.

10. The mold inhibiting product of Claim 9 wherein said third compound is a metal oxide, metal salt, organometallic complex, citric acid, calcium sulfate, triethanol amine or mixtures thereof.

11. The mold inhibiting product of Claim 10, wherein a) said second compound is potassium sorbate, sodium propionate, calcium propionate or mixtures thereof; and b) said third compound is citric acid, zinc oxide, or mixtures thereof.

12. A method of inhibiting mold growth in food stuff, comprising: a) creating said food stuff by mixing the raw ingredients for preparing said food stuff with a mold inhibiting product, said mold inhibiting product comprising: i) a first compound, wherein said first compound is azodicarbonamide; and ii) a second compound, wherein said second compound is citric acid, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and b) exposing said food stuff to a sufficient temperature for a sufficient time to activate said first compound such that said food stuff does not impart an off odor, off flavor or off texture due to the inclusion of said second compound.

13. The method of Claim 12, wherein a) said second compound is potassium sorbate, calcium propionate, sodium propionate or mixtures thereof; b) said temperature is above about 212°F; and c) said mold inhibiting product is present in the amount of about 0.01 to about 20.0 percent by total weight of said raw ingredients for preparing said food stuff.

14. The method of Claim 12, wherein a) said second compound is lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and b) said dry mixture further comprises a third compound for lowering the decomposition temperature of said first compound.

15. The method of Claim 14, wherein a) said second compound is potassium sorbate, calcium propionate, sodium propionate or mixtures thereof; b) said third compound is a metal oxide, metal salt, organometallic complex, citric acid, calcium sulfate, triethanol amine or mixtures thereof; c) said temperature is above about 140°F; and d) said mold inhibiting product is present in the amount of about 0.01 to about 20.0 percent by total weight of said raw ingredients for preparing said food stuff.

16. A method of inhibiting mold growth in food stuff, comprising: a) preparing a mold growth inhibiting product, said mold growth inhibiting product comprising: i) a first compound wherein said first compound is azodicarbonamide; ii) a second compound wherein said second compound is citric acid, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; b) heating said mold growth inhibiting product for a sufficient time and temperature to eliminate a substantial portion of the off odor and taste generally imparted by said second compound; and c) mixing said mold growth inhibiting product with the ingredients used in preparing said food stuff.

17. The method of Claim 16, wherein a) said temperature is about 212°F to about 475°F; b) said time is about 20 to about 30 minutes; and c) said mold inhibiting product is present in the amount of about 0.01 to about 20.0 percent by total weight of said ingredients used in preparing said food stuff.

18. The method of Claim 16, wherein a) said second compound is lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and b) said mold growth inhibiting product further comprises a third compound wherein said third compound is a metal oxide, metal salt, organometallic complex, citric acid, calcium sulfate, triethanol amine or mixtures thereof.

19. The method of Claim 18, wherein a) said second compound is potassium sorbate, calcium propionate, sodium propionate or mixtures thereof; and b) said third compound is zinc oxide, citric acid or mixtures thereof. c) said temperature is above about 140°F; d) said time is about 6 to about 10 minutes; and e) said mold inhibiting product is present in the amount of about 0.01 to about 20.0 percent by total weight of said ingredients used in making said food stuff.

20. A method of preparing a mold growth inhibiting product comprising: a) mixing about 1 part by weight of a dry mixture with about 4 to 8 parts by weight of water to form a first product; wherein said dry mixture is comprised of: i) a first compound present in the amount of about .001 to about 5.0 percent by total weight of said dry mixture, wherein said first compound is azodicarbonamide; and ii) a second compound present in the amount of about 95.0 to about 99.999 percent by total weight of said dry mixture, wherein said second compound is citric acid, lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and b) boiling said first product for about 15 minutes to form a second product; c) cooling said second product to about room temperature; d) filtering said second product; and e) adding an amount of water equivalent to the volume of liquid lost while said first product was boiled to form said mold inhibiting product.

The method of Claim 20, wherein said dry mixture comprises a) about 65.0 to about 99.995 percent of said second compound, wherein said second compound is lactic acid, fumaric acid, potassium sorbate, sodium sorbate, calcium sorbate, sorbic acid, salts of sorbic acid, calcium propionate, potassium propionate, sodium propionate, propionic acid, salts of propionic acid or mixtures thereof; and a third compound present in the amount of about 0.004 to about 30.0 percent by total weight of said dry mixture, wherein said third compound is a metal oxide, metal salt, organometallic complex, citric acid, calcium sulfate, triethanol amine or mixtures thereof.