SI23410A - Antioxidative and antimicrobiological protection of milk and dairy products with extracts of labiateae and their synergistic mixtures - Google Patents

Abstract

The subject of the invention is antioxidative and antimicrobiological protection of milk and dairy products by using extracts from labiateae family plants and their synergistic mixtures. The oil soluble extract of labiateae family plants contains up to 100 wt. % carnosolic acid. The water soluble extract of rosemary contains up to 100 wt. % rosemary acid. The oil soluble extract of labiateae and/or water soluble extract of labiateae or a mixture of labiateae extract and additives (other plant extracts with antioxidative and/or antimicrobiological activity, emulsifiers for applications in food as well as other antioxidants approved in food), which are acting synergistically with the labiateae extract, are added to milk and dairy products in the total active ingredient concentration of minimum 1 mg/kg.

Description

The object of the invention is the antioxidant and antimicrobial protection of milk and milk products. Protection is achieved by plant extracts of the lipid family and their synergistic mixtures. Lips are rosemary, sage, lemon balm, oregano, walleye, mint, thyme and more.

The main active substances in the extracts of plants of the mouthpiece family are camosolic acid, rosemary acid and their derivatives. Camosolic acid is oil-soluble and rosemary acid is a water-soluble active substance.

The lipid extract of plants of the lipid family contains up to 100% by weight of camosolic acid. The water soluble plant extract of the mouthpiece family contains up to 100% by weight of rosemary acid.

The invention relates to the protection of milk and milk products from antioxidant and microbial defects by oil-soluble and / or water-soluble extract of plants of the oral family. The invention further relates to the preparation of mixtures for the antioxidant and antimicrobial protection of milk and milk products based on lip extract and additives, i.e. other plant extracts with antioxidant and / or antimicrobial action, emulsifiers for use in food, and other food-approved antioxidants Oral extracts act synergistically. The combination of lip extract with synergists gives better antioxidant and antimicrobial protection for the product.

Oxidation of milk fat causes the unpleasant odor and taste of milk and milk products and, in addition to lipolysis, which causes hydrolytic irradiation, is one of the most important factors affecting the shelf life of milk and milk products. Dairy products have a complex composition and physicochemical properties and have naturally occurring antioxidants and prooxidants. Milk fat consists mainly of triacylglycerols of 95-96% content, which are found in the milk in the form of fat beads surrounded by a membrane composed of proteins, phospholipids, glycerides, cerebrosides, cholesterol and enzymes. The fatty acid composition of lactic fat is as follows: from 63 to 69% of saturated fatty acids, of which 24% are palmitic and 13% ·

• · stearic, from 27 to 34% of monounsaturated fatty acids, of which 25% is oil and from 2.5 to 3% of polyunsaturated, of which 2% is linoleic fatty acid.

Oxidation of milk fat begins at the phase boundary of the membrane of the fat ball - water and continues in the central triacylglycerol fraction. The appearance of odor and taste after being oxidized is most noticeable in milk, cream and butter because these products are milder in smell and taste.

In addition to oxidation, milk and dairy products are highly susceptible to microbial spoilage. The dairy industry controls the oxidation and microbiological breakdown of milk and milk products in the following ways:

• Low storage temperature, • Oxygen control, • Heat treatment, • Homogenization, and • Proper packaging.

Antioxidant supplementation has been shown to inhibit the occurrence of oxidation of milk and milk products. The use of synthetic antioxidants is banned in many countries. Lipstick extract and blend based on lipstick extract, that is, other plant extracts with antioxidant and / or antimicrobial action, emulsifiers for use in food and other food-approved antioxidants, are a natural alternative to synthetic antioxidants. At the same time, they also contribute to the microbiological protection of milk.

According to the invention, the problem is solved by antioxidant and antimicrobial protection of milk and milk products in the following ways:

Antioxidant and antimicrobial protection of milk and milk products using oil extracts from plants of the oral family. The active substances in the rosemary oil extracts are quarzolic acid and camosol.

Antioxidant and antimicrobial protection of milk and milk products using water-soluble extracts from plants of the oral family. The active substance in water-soluble rosemary extracts is rosemary acid.

Antioxidant and antimicrobial protection of milk and milk products using lip extract and additives (other herbal extracts with antioxidant and / or antimicrobial action, emulsifiers for use in food and other food-approved antioxidants) that act synergistically with lip extract.

Extracts of the plants of the lipid family and their mixtures are diluted with a suitable vehicle, for example, for better distribution by product and more appropriate handling, e.g. edible oil and / or propylene glycol and / or edible salt and / or maltodextrin and / or a diet-approved carrier, optionally added diet-approved emulsifier and used in milk and dairy products.

The addition of lipstick extracts and mixtures thereof in a concentration that varies with the type of milk and milk products does not alter their organoleptic properties. Thermal treatment of milk and thermal processes in the production of dairy products do not affect the efficiency of rosemary extracts and their mixtures.

The invention encompasses antioxidant and antimicrobial protection of milk and milk products using extracts from plants of the oral family and their synergistic mixtures. The lipid extract of plants of the lipid family contains up to 100% by weight of camosolic acid. Water-soluble rosemary extract contains up to 100% by weight of rosemary acid. Lipstick and / or water-soluble lipstick extract and / or a mixture of lipstick extracts and additives (other herbal extracts with antioxidant and / or antimicrobial action, emulsifiers for use in food and other food-approved antioxidants), which with lipid extract in milk and milk products in the total active substance concentration min. 1 mg / kg. Other herbal extracts that synergistically work with lipstick extracts are: green tea extract, citrus extract, naringin-based citrus extract, olive extract, hop extract, carrot extract, guarana extract and others.

The plant extract of the oral family and their synergistic mixtures according to the invention are used in the following ways:

Extract of plants of the mouth or family. its synergistic mixture is added directly to the milk or milk product.

Extract of plants of the mouth or family. its synergistic mixture is put into milk before the dairy product is produced.

Extract of plants of the mouth or family. its synergistic mixture is diluted with a suitable carrier, for example, to better distribute the product and to handle it more appropriately, e.g. with edible oil and / or propylene glycol and / or edible salt and / or maltodextrin and / or other nutritionally authorized carriers, optionally added diet-approved emulsifier and used in milk and dairy products.

The invention will be described with embodiments and illustrations showing:

Figure 1: Results of crude butter rancimat test with added rosemary extract (rosemary extract) at a concentration of 40 mg / kg of camosolic acid, a synergistic mixture based on rosemary extract (MIXTURE) at a concentration of 40 mg / kg of camosolic acid and without additives (CONTRO.

Figure 2: Results of measurement of the acid number of sweet cream with added rosemary extract (Rosemary extract) at a concentration of 40 mg / kg of camosolic acid, a synergistic mixture based on rosemary extract (MIXTURE) at a concentration of 40 mg / kg of camosolic acid and without additives (KONTRO) 15 days of storage at 4 ° C.

Figure 3: Results of TBA measurement of whey concentrate with added rosemary extract (rosemary extract) at a concentration of 40 mg / kg of camosolic acid, a synergistic mixture based on rosemary extract (MIXTURE) at a concentration of 40 mg / kg of camosolic acid and without additives (KONTRO) three weeks of storage at 4 ° C.

Figure 4: Results of TBA measurement of milk powder with added synergistic blend based on rosemary extract (MIXTURE) at a concentration of 40 mg / kg of camosolic acid and without additives (CONTROL) after four months of storage at room temperature.

EXAMPLE 1

Rosemary extract was stirred at a concentration of 0.1% by weight (equivalent to 40 mg / kg of camosolic acid) in the crude butter, which was dissolved in a 40 ° C water bath. We ran the buttercream test concentrate at 100 ° C. Sample with addition of 0,1 wt. % of rosemary extract had 5 times longer induction time * (means 5 times better oxidative stability) than control without additives (CONTROL).

* Rancimat test

With the Rancimat test, the conductive oxidation products of unsaturated fatty acids were measured conductometrically. The result is given as the induction time, that is, the time during which the peroxide number reaches a value of 100 micro eq / kg of fat. The greater the induction time, the more stable the product.

Weigh 3 g of butter into a test tube. The cell was heated to 100 ° C and air was sucked into the sample to accelerate the oxidation. The volatile oxidation products dissolved in water, thus altering the conductivity of the water. It increased sharply when the induction phase was completed.

EXAMPLE 2

The mixture of rosemary extract with tocopherols and emulsifier DATEM (mixture code: MIXTURE) was mixed in concentrations of 0.05 wt% (corresponds to 20 mg / kg of camosolic acid) and 0.1 wt% (corresponds to 40 mg / kg of camosolic acid). raw butter which was dissolved in a 40 ° C water bath. We ran the buttercream test concentrate at 100 ° C. The sample with the addition of 0.05% by weight of the MIXTURE had 9 times longer induction time (means 9 times better oxidative stability) than the control sample without additives (CONTROL). Sample with addition of 0,1 wt. % Of the MIXTURE had an 11-fold longer induction time (meaning 11-fold better oxidative stability) than the control sample without additives.

EXAMPLE 3

Rosemary extract was mixed in sweet cream at a concentration of 0.1% by weight (corresponding to 40 mg / kg of camosolic acid). Sweet cream was stored in the refrigerator at 4 ° C and after 3, 5, 7, 10 and 15 days, the acidity of the sweet cream was measured. After 15 days of feeding, the sample was supplemented with 0.1 wt. % rosemary extract 30% lower acid number * (means 30% better oxidative stability) than the control sample without additives (CONTROL).

* Acid number

The acid number indicates how much mg of KOH is needed to neutralize the free fatty acids contained in 1 g of oil or fat.

Weigh 10 g of the test sample into a flask with a plastic pipette, add 50 ml of ethanol: diethyl ether in a volume ratio of 1: 1 and shake well. Then 3 drops of phenolphthalein solution were added. Titrated with a 0.1 M potassium hydroxide solution until the color went from colorless to slightly pink. We did the same thing with a blind attempt. The acid number (KŠ) was calculated by the following formula:

• · where:

KŠ = (10 * b * f * 0.561) / a

KH - acid number (mg KOH / g fat) a - weigh sample (g) b - consumption (ml) of potassium hydroxide to titrate the sample f - factor 0.1 M potassium hydroxide.

0,561 Factor relating to the molar mass of potassium hydroxide (56,1) and to 1 g of fat when titrated with 0.1 M potassium hydroxide solution of sample (g)

EXAMPLE 4

The mixture of rosemary extract with tocopherols and the emulsifier DATEM (mixture code: MIXTURE) was mixed at a concentration of 0.05 wt% (corresponding to 20 mg / kg of camosolic acid) and 0.1 wt% (corresponding to 40 mg / kg of camosolic acid). sweet cream. Sweet cream was stored in the refrigerator at 4 ° C and after 3, 5, 7, 10 and 15 days, the acidity of the sweet cream was measured. Po

On days 15 of feeding, the sample was supplemented with 0.05 wt. % MIXTURES 56% lower acid number (means 56% better oxidative stability) than control without additives (CONTROL). After 15 days of feeding, the sample was supplemented with 0.1 wt. % of the mixture 57% lower acid number (means 57% better oxidative stability) than the control sample without additives (CONTROL).

EXAMPLE 5

Rosemary extract was mixed in whey concentrate at a concentration of 0.1% by weight (corresponding to 40 mg / kg of camosolic acid) and mixed well. The whey concentrate was stored in the refrigerator at 4 ° C and after 1, 2 and 3 weeks the optical density of the whey concentrate was measured by TBA assay. After 3 weeks of feeding, the sample was supplemented with 0.1 wt. % rosemary extract 69% lower optical density * (means 69% better oxidative stability) than the control without additives (CONTROL).

* Determination of optical density by TBA test

TBA test is an empirical method for determining the degree of oxidation in fats and fatty foods. The test indicates the level of fat in the aldehydes present. Thiobarbitum acid reacts specifically with malonaldehyde (MDA) to give a red chromogen, which is determined spectrophotometrically. The result is given as the optical density measured at a wavelength of 532 nm. Lower optical density means a more oxidatively stable product.

17.6 ml of whey concentrate was pipetted into a conical flask, heated to 30 ° C in a water bath, 1 ml of trichloroacetic acid and 2 ml of 95 wt% ethanol were added, stoppered and shaken for 10 seconds. After five minutes, the contents were filtered through filter paper. To four ml of pure filtrate was added 1 ml of TBA solution, which was obtained by dissolving 1.4 g of 2-thiobarbitum acid in 95% by weight ethanol to 100 ml. The filtrate tube was capped, stirred and heated in a 60 ° C water bath for 60 minutes. The reference sample was prepared in the same manner except that 4 ml of distilled water was pipetted into the tube instead of the filtrate. The sample and reference sample were cooled after incubation and the optical density (D) was measured at 532 nm.

EXAMPLE 6

The mixture of rosemary extract with tocopherols and the DATEM emulsifier (mixture code; MIXTURE) was mixed at a concentration of 0.05 wt% (corresponding to 20 mg / kg of camosolic acid) and 0.1 wt% (corresponding to 40 mg / kg of carnosolic acid). whey concentrate and mix well. The whey concentrate was stored in the refrigerator at 4 ° C and after 1, 2 and 3 weeks the optical density of the whey concentrate was measured by TBA assay. After 3 weeks of feeding, the sample was 0.05 wt. % of the mixture 52% lower optical density (52% better oxidative stability) than the control sample without additives (CONTROL). After 3 weeks of feeding, the sample was supplemented with 0.1 wt. % of the mixture 70% lower optical density (70% better oxidative stability) than the control sample without additives (CONTROL).

EXAMPLE 7

Pasteurized milk with standardized milk fat is 0.1 wt. % (corresponds to 40 mg / kg of camosolic acid) with respect to the final product (milk powder) added a mixture of rosemary extract with tocopherols and an emulsifier DATEM (mixture code: MIXTURE) before the milk concentration process and mixed well.

This was followed by a process of thickening the milk in a multi-stage evaporator, in which the milk was heated to approx. 95 ° C. Due to the pressure in the evaporators, the temperature was lowered from the beginning to the end of the process, so that the outlet temperature was 45-47 ° C. The milk thickened in the evaporators from the initial 12% of dry matter to approx. 47 - 48% of dry matter.

The process of milk thickening was followed by a drying process in which concentrated high-pressure milk was pumped into a drying tower where it dispersed before entering. The drying temperature in the drying tower was 190 - 200 ° C. The powdered milk is then sown in e.g. the instantizer was dried to the desired final moisture content and cooled and packaged in suitable packaging.

After production, the content of camosolic acid was determined using high performance liquid chromatography (HPLC) and the use of an electrochemical detector. The content of camosolic acid in the milk powder corresponded to the value at dosage, which means that the active substance is stable during the milk powder production process.

For comparison, we prepared a sample of milk powder without additives (CONTROL) from the same batch of pasteurized milk and following the same procedure.

The powdered milk was stored at room temperature and after 1, 2, 3 and 4 months the optical density of the milk powder concentrate was measured by TBA test. After 4 months of feeding, the sample was supplemented with 0.1 wt. % of the mixture 65% lower optical density (means 65% better oxidative stability) * than the control without additives (CONTROL).

After 4 months of feeding, microbiological evaluation of both milk powder samples was also performed. In the powder-free milk (CONTROL), 15 CFU / g of Bacillus cereus was present, in the sample with the addition of a MIXTURE at a concentration of 0.1% by weight, this bacterium was not present. The results clearly show that the addition of a mixture of rosemary extract with tocopherols and an emulsifier DATEM (mixture code: MIXTURE) inhibits the growth of Bacillus cereus in milk powder.

Also, the total number of microorganisms in milk with the addition of a mixture of rosemary extract with tocopherols and an emulsifier DATEM (mixture code: MIXTURE) was 5 times lower than in the case of the control sample (CONTROL). The results of the microbiological evaluation of milk powder after 4 months of storage at room temperature are shown in Table 1.

• · · · ·

Table 1: Results of microbiological evaluation of milk powder with the addition of a mixture of rosemary extract with tocopherols and a DATEM emulsifier (mixture code: MIXTURE) and a control sample (CONTROL).

The parameter The result CONTROL MIXTURE in conc. 0.1 wt.% Salmonella spp. not found in 25 g not found in 25 g Bacillus cereus 15 CFU / g <10 CFU / g Coliform bacteria <10 CFU / g <10 CFU / g Enterobacterriaceae <10 CFU / g <10 CFU / g Yeast <10 CFU / g <10 CFU / g Mold <10 CFU / g <10 CFU / g Aerobic mesophilic bacteria 1000 CFU / g 200 CFU / g Escherichia coli not found in 1 g not found in 1 g

* Determination of optical density by TBA test

The milk powder was dissolved in lukewarm water, the weight ratio was milk powder: water was 12.5: 87.5. The following procedure was identical to the procedure of EXAMPLE 5.

These examples also apply to the antioxidant extracts of other herbs such as rosemary, sage, lemon balm, oregano, walnut, mint, thyme and others.

The antioxidant and antimicrobial protection of milk and milk products according to the invention is therefore characterized by the fact that lipstick extracts and their synergistic mixtures are added to milk and milk products. Substances that act synergistically with the lip extract are: other herbal extracts with antioxidant and / or antimicrobial action, emulsifiers for use in food, and other food approved antioxidants. Extracts from plants of the oral family are added to milk and dairy products, namely rosemary oil extract containing up to 100% by weight of camosolic acid and / or water-soluble rosemary extract containing up to 100% by weight of rosemary acid or a mixture of oil-soluble and / or water-soluble extract rosemary and / or additives synergistically acting at a concentration of min. 1 mg / kg total active ingredients. The plant extracts of the oral family and their synergistic mixtures are added directly to the milk or milk product or to the milk before the milk product is produced. The plant extracts of the mouthpiece family and mixtures thereof are diluted with a suitable carrier and / or emulsifier, preferably edible oil and / or propylene glycol and / or edible salt and / or maltodextrin and / or a dietary carrier.

The addition of rosemary extracts and mixtures thereof does not alter the organoleptic properties of milk and milk products. The thermal treatment of milk and milk products and the thermal processes in the production of milk and milk products do not affect the efficiency of rosemary extracts and mixtures thereof.

Claims (7)

PATENT APPLICATIONS Antioxidant and antimicrobial protection of milk and milk products, characterized in that the extracts of the mouthpieces and their synergistic mixtures are added to the milk and milk products. Protection according to claim 1, characterized in that the substances which act synergistically with the lipstick extract are: other plant extracts with antioxidant and / or antimicrobial action, emulsifiers for use in food and other food-approved antioxidants. Protection according to claim 1, characterized in that extracts from plants of the oral family are added to milk and dairy products, namely, rosemary oil extract containing up to 100% by weight of camosolic acid and / or water-soluble rosemary extract containing up to 100 wt of rosemary acid or a mixture of oil - soluble and / or water - soluble rosemary extract and / or additives which synergistically act at a concentration of min. 1 mg / kg total active ingredients. Protection according to claim 1, characterized in that the plant extracts of the lipid family and their synergistic mixtures are added directly to the milk or the milk product or to the milk before the milk product is produced. Protection according to claim 1, characterized in that the extracts of the plants of the oral family and mixtures thereof are diluted with a suitable carrier and / or emulsifier, preferably edible oil and / or propylene glycol and / or edible salt and / or maltodextrin and / or others in diet allowed carrier. Protection according to claim 1, characterized in that the addition of rosemary extracts and mixtures thereof does not alter the organoleptic properties of milk and milk products. Protection according to claim 1, characterized in that the thermal treatment of milk and milk products and the thermal processes in the production of milk and milk products do not affect the performance of rosemary extracts and mixtures thereof.