阅读说明：本技术 降低uht灭菌乳脂肪上浮程度和投诉率的方法 (Method for reducing UHT sterilized milk fat floating degree and complaint rate ) 是由 庄超超 郭占辉 于 2019-11-29 设计创作，主要内容包括：本发明提供了一种降低UHT灭菌乳脂肪上浮程度和投诉率的方法,该方法包括对牛奶进行蛋白稳定处理和灭菌处理的操作,其中,所述蛋白稳定处理的温度为90-95℃,时间为110-130s,所述灭菌处理包括在蛋白稳定处理后升温至140℃、在140℃保持4s、再由140℃降温至121.1℃的操作。本发明还提供了一种由上述制备方法得到的UHT灭菌乳,其中,所述UHT灭菌乳的蛋白酶活性为100-140u/100ml、糠氨酸含量为130-150mg/100g蛋白质。本发明提供的方法能够提高灭菌效率、改善产品在货架期内发生的脂肪上浮现象、减少酸包、苦包、结块现象的发生,降低投诉率。(The invention provides a method for reducing the floating degree and complaint rate of UHT sterilized milk fat, which comprises the operation of protein stabilization treatment and sterilization treatment on milk, wherein the temperature of the protein stabilization treatment is 90-95 ℃ and the time is 110-130s, and the sterilization treatment comprises the operation of heating to 140 ℃, keeping at 140 ℃ for 4s and then cooling from 140 ℃ to 121.1 ℃ after the protein stabilization treatment. The invention also provides UHT sterilized milk obtained by the preparation method, wherein the protease activity of the UHT sterilized milk is 140u/100ml, and the content of the furosine is 130-150mg/100g protein. The method provided by the invention can improve the sterilization efficiency, improve the fat floating phenomenon of the product in the shelf life, reduce the occurrence of acid package, bitter package and caking phenomenon, and reduce the complaint rate.)

1. A method for reducing the floating degree and complaint rate of UHT sterilized milk fat comprises the operations of protein stabilization treatment and sterilization treatment on milk, wherein the temperature of the protein stabilization treatment is 90-95 ℃ and the time is 110-130s, and the sterilization treatment comprises the operations of heating to 140 ℃, keeping at 140 ℃ for 4s and then cooling from 140 ℃ to 121.1 ℃ after the protein stabilization treatment.

2. The method of claim 1, wherein the protein stabilization treatment is at a temperature of 94.5 ℃ for 120 s.

3. Method according to claim 1 or 2, wherein the sterilization treatment comprises the following processes: firstly, heating from 94.5 ℃ to 121.4 ℃; then raising the temperature from 121.4 ℃ to 140 ℃; then keeping the temperature at 140 ℃ for 4s, and finally reducing the temperature from 140 ℃ to 121.1 ℃.

4. A method according to claim 1 or 3, wherein the sterilization process comprises the following processes: firstly, heating from 94.5 ℃ to 121.4 ℃ and consuming 33.62 s; then raising the temperature from 121.4 ℃ to 140 ℃ and consuming 17.44 s; then the temperature is kept at 140 ℃ for 4s, and finally the temperature is reduced to 121.1 ℃ for 14.22s, so that the heat treatment is completed.

5. A preparation method of UHT sterilized milk comprises the steps of milk collection, standardization, pasteurization, semi-finished product preparation, heat treatment and filling,

wherein the heat treatment step comprises protein stabilization treatment and sterilization treatment, the temperature of the protein stabilization treatment is 90-95 ℃, the time is 110-130s, and the sterilization treatment comprises the operation of raising the temperature to 140 ℃, keeping the temperature at 140 ℃ for 4s and then reducing the temperature from 140 ℃ to 121.1 ℃ after the protein stabilization treatment.

6. The method according to claim 5, wherein the temperature of the protein stabilization treatment is 94.5 ℃ and the time is 120 s.

7. The production method according to claim 5, wherein the sterilization treatment includes the following processes: the temperature is raised from 94.5 ℃ to 121.4 ℃, then from 121.4 ℃ to 140 ℃, then kept at 140 ℃ for 4s, and finally lowered from 140 ℃ to 121.1 ℃.

8. The production method according to claim 5, wherein the heat treatment includes the following process: firstly, heating from 94.5 ℃ to 121.4 ℃ and consuming 33.62 s; then raising the temperature from 121.4 ℃ to 140 ℃ and consuming 17.44 s; then keeping at 140 ℃ for 4s, and finally cooling from 140 ℃ to 121.1 ℃ for 14.22 s.

9. The method of claim 5, wherein in the step of standardisation and pasteurisation, the pasteurisation temperature is between 80 and 90 ℃ for a time of 15 s.

10. A UHT sterilized milk obtained by the preparation method of any one of claims 5 to 9, wherein the protease activity of the UHT sterilized milk is 140u/100ml, and the content of the furosine is 130-150mg/100g protein.

Technical Field

The invention relates to a heat treatment process of UHT sterilized milk, in particular to a method for reducing the fat floating degree and the complaint rate of the UHT sterilized milk, the UHT sterilized milk and a preparation method thereof.

Background

The proportion of UHT sterilized milk in the consumption of liquid milk in China is continuously increased, and the UHT sterilized milk plays an increasingly important role in the dietary culture of people. Compared with the requirement of pasteurized low-temperature milk on a cold chain, the shelf life of the pasteurized low-temperature milk is usually only about 7 days, the UHT milk solves the problem that the liquid milk is difficult to transport, store and keep fresh, the shelf life of the UHT milk can reach 6-12 months, and nutrient substances are effectively kept. On the other hand, the nutrient substances in the milk comprise protein, fat, lactose, vitamins, minerals and the like, are easy to digest and absorb, and are suitable for almost all people except infants and lactose intolerance people.

Bacillus is one of the common genera in raw milk. For climatic reasons, the genera Bacillus, lactococcus, Acinetobacter, and Pseudomonas compete with one another throughout the year, forming a balance. In summer, in particular, bacillus predominates. Wherein spores generated by the heat-resistant bacillus are stable to heat and are not easy to be killed by high temperature. The UHT design aims at killing heat-resistant spores such as spores of stearothermophilus, bacillus subtilis, and spores of waxy products, and stipulates the minimum requirement that the sterilization efficiency F0 is 9. Commercial aseptic products were produced despite UHT sterilization efficiencies of F0 to a value of 9. However, practice has shown that heat-resistant spores remain in UHT-heat-treated sterilized pure milk, and the F0 value required for killing these heat-resistant spores is higher than 9. Meanwhile, during the shelf life, the possibility of germination of the heat-resistant spores remained in the product often causes consumer complaints of acid bags, bitter bags and caking.

According to the identification of reconstituted milk in pasteurized milk and UHT sterilized milk in the national agricultural industry standard, when the lactulose of the UHT sterilized milk is less than 600.0mg/L, the furosine is more than 190.0mg/100g of protein and the ratio of the lactulose to the furosine is less than 1.80, the UHT sterilized milk is judged to contain the reconstituted milk. Due to the fact that the risk of extracting and detecting reconstituted milk by the state is reduced, the heat treatment intensity of UHT sterilized pure milk is reduced, and the probability and risk of heat-resistant spores remaining in UHT sterilized milk are increased.

In addition, UHT sterilized milk is prone to fat floating during shelf life, especially after 5-6 months of storage. This is also directly related to insufficient UHT heat treatment strength. Fat is the main source of the unique flavor of milk, and the floating of fat to a certain extent also means fat oxidation. Therefore, fat floating is not only an expression of non-uniform tissue state but also deteriorates taste and flavor, and is likely to cause misunderstanding of consumers and complaints.

For many years, fatty acid monoglyceride has been added to the formula of pure milk, and the good surface activity of the fatty acid monoglyceride is utilized as an emulsifier to stabilize the texture state of the milk. Nowadays, as the consumers continuously pursue the quality, more and more consumers want pure milk without adding any substance, which also presents more challenges to manufacturers, and needs to be improved in the process in order to obtain the uniform and stable state of pure milk in 6 months of shelf life.

Disclosure of Invention

In order to solve the problems, the invention aims to provide a method for reducing the fat floating degree and the complaint rate of UHT sterilized milk, UHT sterilized milk and a preparation method thereof. The method provided by the invention can improve the sterilization efficiency on the premise of ensuring that the content of the furosine in the product meets the standard, reduce the complaint rate of the product caused by acid package, bitter package and caking phenomena in the shelf life, improve the fat floating phenomenon of the UHT sterilized milk in the shelf life, and improve the stability of the UHT sterilized milk product.

The invention provides a method for reducing the floating degree and complaint rate of UHT sterilized milk fat, which comprises the operation of protein stabilization treatment and heat treatment on milk, wherein the temperature of the protein stabilization treatment is controlled to be 90-95 ℃, and the time is controlled to be 110-130s, so that the germination of heat-resistant spores remained in the milk is favorably induced, and the heat-resistant spores are conveniently killed; the sterilization treatment comprises the operation of raising the temperature to 140 ℃ after the protein stabilization treatment and keeping the temperature at 140 ℃ for 4s, thereby effectively killing heat-resistant spores on the premise of ensuring that the furosine does not exceed the standard.

The invention also provides a preparation method of the UHT sterilized milk, which comprises the steps of milk collection, standardization, pasteurization, semi-finished product preparation, heat treatment and filling, wherein the heat treatment step comprises protein stabilization treatment and sterilization treatment, the temperature for protein stabilization is 90-95 ℃, and the time is 110-130 s; the sterilization treatment comprises the operations of raising the temperature to 140 ℃ after the protein stabilization treatment, keeping the temperature at 140 ℃ for 4s, and then lowering the temperature from 140 ℃ to 121.1 ℃.

In the research process, 335 batches of UHT sterilized milk sold in the market are collected, bacillus cereus MPN method in GB4789.14-2014 is used for detecting the bacillus cereus residue, 48 batches of bacillus cereus residues are detected, the detection rate is 14.33%, and the bacillus cereus, the thuringiensis and the bacillus mycoides are mainly biochemically identified. However, the inventor finds that spores which are still unidentified and more heat-resistant may remain in the milk compared with the three spores, and if the spores germinate in the shelf life, the spores are easy to cause phenomena of acid package, bitter package and caking, so that the complaint rate of consumers is increased. Practice shows that the three complaints are easier to occur in the milk produced in summer, which is consistent with the rule that the bacillus is dominant in the raw milk flora in summer.

According to the preparation method provided by the invention, protein stabilizing treatment is added before sterilization treatment in the UHT heat treatment process, so that favorable conditions are provided for heat-resistant spore germination, the germination efficiency of the heat-resistant spores is improved (the germination efficiency of the heat-resistant spores is induced by greatly stimulating nutrient molecules, the germination time of the heat-resistant spores is shortened, the death rate of the heat-resistant spores after germination is increased), and the heat-resistant spores are promoted to enter a state of germination and being incapable of tolerating sterilization treatment; meanwhile, the highest temperature of the sterilization treatment is set to be more than 115 ℃, the sterilization efficiency of the process is effectively improved, and from about 115 ℃, the lethal efficiency of the heat-resistant spores is rapidly increased along with the increase of the temperature, so that the heat treatment temperature adopted by the invention can kill the heat-resistant spores in the germination period and reduce the content of the heat-resistant spores in the UHT sterilized milk.

Further research of the invention finds that the degree of fat floating of UHT sterilized milk in shelf life is also closely related to the UHT heat treatment process. Protein molecules in milk can disperse and interact between oil-water interfaces to form a viscous continuous phase surrounding oil droplets, which plays an important role in stabilizing the tissue state. Since milk is a good medium for microorganisms, it is stored at 4-6 ℃ from milking to the factory, which inevitably results in the presence of psychrophilic bacteria dominating the milk storage process. Meanwhile, psychrophiles represented by Pseudomonas grow to produce heat-resistant enzymes, and Table 1 lists some of the heat-resistant enzymes secreted by Pseudomonas. In addition, the milk has certain natural protease, mainly plasmin, mainly derived from blood, has certain heat resistance, and can still retain certain activity after sterilization. Thermostable enzymes, especially proteases, are capable of hydrolyzing alpha-casein, beta-casein, destroying the surface structure of milk fat globules and casein, causing fat to bind to fat, fat to casein and aggregate, forming small flakes floating on the upper part of milk, reducing the stability of milk fat.

TABLE 1 Thermosidase production by Pseudomonas

Enzyme type	Temperature of	Time s	Residual activity%
				Pseudomonas fluorescens P26	149	90	0
Pseudomonas fluorescens 22F	150	288	0
				Pseudomonas MC50	100	63	0
Ps.fluorescens CY091	100	600	20
				Pseudomonas fluorescens B52	149	30	60
Pseudomonas fluorescens 189	149	30	56
				Pseudomonas fluorescens B12	149	30	27
Pseudomonas fluorescens 51	149	30	10
				Pseudomonas fluorescens 53	149	30	35

The invention selects the content of the furfuryl acid and the content of the protease as indexes for measuring the heat treatment strength, and compared with the F0 value, the content of the furfuryl acid and the content of the protease can more accurately evaluate the heat treatment strength in the preparation process of the UHT sterilized milk. In the process of preparing UHT sterilized milk, the aim of reducing enzyme activity is generally achieved by adopting reasonable combination of temperature and time for heat treatment, wherein UHT sterilization is the most important link in the heat treatment. The F0 value, the furfuryl acid content and the protease activity were all correlated with the intensity of the heat treatment. However, the F0 value is only a measure of the strength of UHT heat treatment; the content of the furosine is used for indicating the degree of the nutritional ingredients of the milk damaged by heat, and simultaneously can reflect the heat treatment strength; the protease activity is similar to the content of the furosine, and can reflect the heat treatment intensity of the milk in the whole processing link, particularly pasteurization and UHT heat treatment, and the protease is also a main factor influencing fat floating. The research of the invention finds that the product which generates fat floating has higher protease level and lower furosine level, namely, the heat treatment intensity is lower, and the inactivation effect on enzymes is weak.

The invention can inactivate the protease activity in the milk and fully denature the whey protein by adding protein stabilization treatment in the heat treatment process, including heat preservation at 90-95 ℃ for 110-130s, thereby avoiding the occurrence of fat floating. For the inactivation of the activity of enzymes (such as protease), the effect of the heating time in the heat treatment process is more obvious than the effect of the heating temperature, and the temperature of the protein stabilizing treatment adopted by the invention can fully inactivate the enzymes, particularly the protease. In the actual production process, the temperature range capable of realizing long-time heat preservation is basically 90-105 ℃, and higher temperature can cause the furfuryl acid level to rise rapidly, thereby causing the loss of nutrient components. In addition, the temperature of 90-95 ℃ protein stabilization treatment adopted by the invention can also ensure that the lactalbumin can be combined with casein after being fully denatured to form a more stable macromolecular structure, so that the capability of enzyme-catalyzed decomposition of protein is reduced, the fat globule membrane is not easy to be damaged, and the degree of fat floating is reduced.

According to an embodiment of the present invention, the temperature of the protein stabilization treatment can be controlled to 94.5 ℃ for 120 seconds.

In some embodiments, the sterilization treatment may be performed according to the following process: firstly, heating from 94.5 ℃ to 121.4 ℃; then raising the temperature from 121.4 ℃ to 140 ℃ for s; then keeping the temperature at 140 ℃ for 4s, and finally reducing the temperature from 140 ℃ to 121.1 ℃. Preferably, the time taken to raise the temperature from 94.5 ℃ to 121.4 ℃ is controlled to be 33.62s, the time taken to raise the temperature from 121.4 ℃ to 140 ℃ is controlled to be 17.44s, and the time taken to lower the temperature from 140 ℃ to 121.1 ℃ is controlled to be 14.22 s.

According to an embodiment of the present invention, the pasteurization temperature may be controlled to 80-90 ℃ and the time may be controlled to 15 seconds in the standardization and pasteurization step.

According to a particular embodiment of the invention, the process for the preparation of UHT sterilized milk may comprise the steps of:

1. milk recovery: collecting milk detected by raw milk at 1-8 deg.C, filtering, cooling, and storing;

2. standardization and pasteurization: preheating milk to 55-65 deg.C, centrifuging at 4700-4900 rpm, homogenizing at 30/180bar and 55-65 deg.C, flash evaporating at 55-75 deg.C and 0-0.3bar, pasteurizing at 80-90 deg.C for 15s, and cooling to 1-8 deg.C;

3. preparing a semi-finished product: stirring sterilized milk at 940r/min, and cooling to 1-8 deg.C;

4. protein stabilization: keeping degassed (-0.35bar to-0.8 bar) and homogenized (70-75 deg.C, 50/250bar) milk at 90-95 deg.C (preferably 94.5 deg.C) for 110-130s (preferably 120 s);

5. and (3) sterilization treatment: sterilizing the heat-preserved milk at 140 deg.C for 4s (preferably heating from 94.5 deg.C for 33.62s to 121.4 deg.C, heating from 121.4 deg.C for 17.44s to 140 deg.C, and maintaining at 140 deg.C for 4 s);

6. filling: and cooling the sterilized milk to below 30 ℃, aseptically filling, and taking out after the milk is detected to be qualified to obtain the UHT sterilized milk.

The invention also provides UHT sterilized milk which is obtained by the preparation method, wherein the protease activity of the UHT sterilized milk is 140u/100ml, and the content of the furosine is 150mg/100g protein.

The invention has the beneficial effects that:

1. the method provided by the invention combines protein stabilization treatment and sterilization treatment, improves the sterilization efficiency while ensuring that the content of the furosine does not exceed the standard, reduces the occurrence of acid package, bitter package and caking and reduces the complaint rate.

2. The method provided by the invention adds protein stabilizing treatment before heat treatment, is beneficial to the inactivation of enzyme activity, and avoids the floating of fat in the product.

Drawings

FIG. 1 is a boxplot of the protease activity of the products of comparative example 1 and example 1.

FIG. 2 shows the results of testing the content of furfuryl acid in the products of comparative example 1 and example 1.

Detailed Description

The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.

Comparative example 1

The comparative example provides a preparation method of conventional UHT sterilized milk, which specifically comprises the following steps:

1. milk recovery: collecting milk detected by raw milk at 1-8 deg.C, filtering, cooling, and storing;

2. standardization and pasteurization: preheating milk to 55-65 deg.C, centrifuging at 4700 and 4900 rpm, homogenizing at 30/180bar and 55-65 bar, flash evaporating at 55-75 deg.C and 0-0.3bar, pasteurizing at 80-90 deg.C for 15s, and cooling to 1-8 deg.C;

3. preparing a semi-finished product: stirring sterilized milk at 940r/min, and cooling to 1-8 deg.C;

4. and (3) sterilization treatment: heating degassed (-0.35bar to-0.8 bar) and homogenized (70-75 deg.C, 50/250bar) milk at 94.5 deg.C for 33.62s to 121.4 deg.C, heating at 121.4 deg.C for 17.44s to 139 deg.C, maintaining at 139 deg.C for 4s, cooling from 139 deg.C to 121.1 deg.C, and consuming 14.22 s;

5. filling: and cooling the sterilized milk to below 30 ℃, aseptically filling, and taking out after the milk is detected to be qualified to obtain the UHT sterilized milk product.

The heat treatment process used in this comparative example is summarized in table 2, and table 3 shows the types of tubes used in the heat treatment process.

TABLE 2

Heat treatment process	Temperature change	Heat treatment time (unit: second)
			12-section milk water heat exchange tube nest	Uniformly raising the temperature from 94.5 ℃ to 121.4 DEG C	33.62
10-section milk water heat exchange tube nest	Raising the temperature from 121.4 ℃ to 139 ℃ at a constant speed	17.44
			Sterilization maintenance section	Keeping the temperature at 139 DEG C	4

TABLE 3

Heat treatment process	Number of tubes	Tubular type
			12-section milk water heat exchange tube nest	12 sections, each section being about 3.32 m long	The internal diameter of the tubule is 16mm, and the tubule contains 14 tubules
10-section milk water heat exchange tube nest	10 sections, each section is about 3.15 meters long	The internal diameter of the tubule is 14mm, and the tubule contains 12 tubules
			Sterilization maintenance section	1 section, about 6.80m long	Inner diameter of 50mm

Example 1

This example provides a method for preparing UHT sterilized milk, comprising the steps of:

1. milk recovery: collecting milk detected by raw milk at 1-8 deg.C, filtering, cooling, and storing;

2. standardization and pasteurization: preheating milk to 55-65 deg.C, centrifuging at 4700-4900 rpm, homogenizing at 30/180bar and 55-65 deg.C, flash evaporating at 55-75 deg.C and 0-0.3bar, pasteurizing at 80-90 deg.C for 15s, and cooling to 1-8 deg.C;

3. preparing a semi-finished product: stirring sterilized milk at 940r/min, and cooling to 1-8 deg.C;

4. protein stabilization: maintaining degassed (-0.35bar to-0.8 bar) and homogenized (70-75 deg.C, 50/250bar) milk at 94.5 deg.C for 120 s;

5. and (3) sterilization treatment: heating the preserved milk from 94.5 ℃ to 121.4 ℃ for 33.62 seconds, heating from 121.4 ℃ to 140 ℃ for 17.44 seconds, keeping the temperature at 140 ℃ for 4 seconds, and cooling from 140 ℃ to 121.1 ℃ for 14.22 seconds;

6. filling: and cooling the sterilized milk to below 30 ℃, aseptically filling, and taking out after the milk is detected to be qualified to obtain the UHT sterilized milk product.

This example was modified from the thermal treatment equipment used in comparative example 1 by measuring the temperature of UHT different tube arrays using a thermometer, welding at 94.5 c using about 4-5 meters DN50 food grade 316 stainless steel tube, 4 slip knots, 4-5 bends and connecting to an incubator. The heat treatment process used in this comparative example is summarized in table 4. Table 5 shows the types of tubulation used in the heat treatment process of this example.

TABLE 4

Heat treatment process	Temperature change	Heat treatment time (unit: second)
			Protein stabilizing segment	Maintain about 94.5 deg.C	120
12-section milk water heat exchange tube nest	Uniformly raising the temperature from 94.5 ℃ to 121.4 DEG C	33.62
			10-section milk water heat exchange tube nest	Raising the temperature from 121.4 ℃ to 140 ℃ at a constant speed	17.44
Sterilization maintenance section	Keeping the temperature at 140 DEG C	4

TABLE 5

Heat treatment process	Number of tubes	Tubular type
			Protein stabilizing segment	1 section, about 203.8 m long	Inner diameter of 50mm
12-section milk water heat exchange tube nest	12 sections, each section being about 3.32 m long	The internal diameter of the tubule is 16mm, and the tubule contains 14 tubules
			10-section milk water heat exchange tube nest	10 sections, each section is about 3.15 meters long	The internal diameter of the tubule is 14mm, and the tubule contains 12 tubules
Sterilization maintenance section	1 section, about 6.80m long	Inner diameter of 50mm

In the present embodiment, the time used in each temperature stage of the heat treatment is calculated, and the calculation method is exemplified by 12 sections of milk-water heat exchange tubes.

12-section milk water heat exchange tube attribute: contains 14 small tubes with the inner diameter of 16 mm. The flow rate of the milk is flow/sectional area, so that the time for the milk to flow through the transformed 12 sections of milk water heat exchange tubes is calculated, and each tube section is 3.32 meters long.

Similarly, the time for the milk to flow through the 10-section milk water heat exchange tube array and the sterilization holding section can be calculated according to the method in the table 4.

The sterilization efficiency of the sterilization treatment of this example was calculated as follows:

the sterilization treatment process in the preparation method provided by this embodiment is as follows: 33.62 seconds are consumed when the milk is uniformly raised from 94.5 ℃ to 121.4 ℃, 17.44 seconds are consumed when the milk is uniformly raised from 121.4 ℃ to 140 ℃, 4 seconds are maintained at 140 ℃, and 14.22 seconds are consumed when the milk is uniformly lowered from 140 ℃ to 121.1 ℃. The temperature of more than 121.1 ℃ is an effective starting point of the sterilization efficiency, and the UHT overall sterilization efficiency is calculated according to a formula, namely the UHT overall sterilization efficiency is realized by calculating the area which is formed by 0.37 second consumed by 121.1-121.4 ℃, 17.44 seconds consumed by 121.4-140 ℃, 4 seconds consumed by 140 ℃ and 14.22 seconds consumed by reducing the temperature of 140 ℃ to 121.1 ℃.

Taking 17.44 seconds consumed by 121.4-140 ℃ as an example, the calculation process is as follows:

where T is time and T is temperature.

Order to

Then

Calculated, F0 ═ 5.1955

Similarly, the calculation results of the remaining stages are summarized in table 6:

TABLE 6

The total sterilization efficiency F0 of the heat treatment process in the production method provided in comparative example 1 was calculated according to the above method, and the calculation results are summarized in table 7:

TABLE 7

The total sterilization efficiency F0 during the heat treatment of example 1 was calculated to be 14.54 and the total sterilization efficiency F0 during the heat treatment of comparative example 1 was calculated to be 11.95. Compared with the F0 value, the preparation method provided by the invention can greatly improve the sterilization efficiency of the UHT sterilized milk, is more favorable for killing heat-resistant spores and reducing the residue of the spores in the UHT sterilized milk, thereby reducing the acid-coated, bitter-coated and caking situations of the UHT sterilized milk in the shelf life and reducing the complaint rate.

Test example 1 product quality test

The quality detection of the UHT sterilized milk with long shelf life prepared in the example 1 is carried out, and the specific method comprises the following steps: the whole indexes of the product which is just delivered from the factory are detected, and a centrifugal experiment (precipitation) and a boiling experiment are respectively carried out.

The specific process of centrifugation is as follows: 30ml of the product prepared in example 1 was centrifuged at 4000 rpm for 20min, the supernatant was removed, the volume of the remaining precipitate was read, and it was determined that the precipitate volume was equal to or less than 0.1ml, normal, and the precipitate volume was greater than 0.1ml, abnormal, and the product of example 1 had a precipitate volume within the normal range.

The specific process of boiling is as follows: 50ml of the product prepared in example 1 is taken and heated on an electric hot plate or an electric ceramic furnace while shaking until boiling, and then cooled to 70-80 ℃, and then a tester smells whether the smell meets the quality standard requirement (no smell is required), and checks whether the tissue state of the boiled product meets the standard requirement (the requirement is that the boiled product is in a uniform state, no precipitate, no clot and no visible mechanical impurities with normal vision). The product of example 1 was normal in both odor and texture.

This test example also performed a number of routine tests on the product prepared in example 1. Wherein fat (unit g/100g), protein (unit g/100g), whole milk solids (unit g/100g) and pH are measured by an instrument; the color, taste and smell, the tissue state and the taste are classified into evaluation by professional sensory evaluating personnel; alcohol is determined by rapid chemical test; acidity (unit ° T), nitrate, nitrite were determined according to GB 5009.239-2016; the degree of impurities (in mg/8L) was determined according to GB 5413.30-2016.

The test results show that all indexes of the product prepared in example 1 are normal, and the test results are summarized in table 8. The alcohol test result "75-" in table 8 indicates that the acidity of the sample can pass the test of 75% alcohol test, and the sample acidity is qualified.

TABLE 8

Test example 2 complaint Rate

The complaints of sourness, bitterness and caking of the UHT-sterilized milks prepared in comparative example 1 and example 1 are shown in table 9, and it can be seen that the complaint of the UHT-sterilized milks prepared in example 1 is reduced by 6.58% as compared with comparative example 1.

TABLE 9

Test example 3 fat-floating yield

Table 10 shows the fat-lifting yield statistics for the products of comparative example 1 and example 1. It is defined in the industry that after 6 months of storage at normal temperature, namely after the shelf life, the thickness of the box cover fat of the sterilized milk is more than 3 mm, namely, unqualified fat floats upwards. As can be seen from table 10, the fat-floating yield of the product prepared in example 1 was improved by 9% compared to comparative example 1.

Watch 10

Test example 4 protease Activity test

The commonly used method for detecting the protease activity is the "Folin phenol method". In order to make the detection result more accurate, the products prepared in example 1 and comparative example 1 were respectively kept at 37 ℃ for 7 days before the test, so that the inactivated protease in the finished product recovers activity as much as possible, and then the protease activity values were detected and compared by a double sample T test, thereby avoiding the problem of poor reproducibility of the method (the inactivated heat-resistant protease may be reactivated under external stimuli such as high temperature exposure if the finished product is impacted during storage). FIG. 1 is a boxplot of the protease activity of the products of comparative example 1 and example 1, and Table 11 is the results of the two-sample T test of the product of example 1 and the product of comparative example 1. As can be seen from fig. 1 and table 11, the average level of protease activity of the product of comparative example 1 is 257.1u/100ml, and the average level of protease activity of the product of example 1 is 120.4u/100ml, which are significantly different (p ═ 0.012), thus proving that the protease activity can be effectively inactivated by the method provided by the present invention.

Table 11 double sample T-test of comparative example 1 and example 1 products

	N	Mean value	Standard deviation of	Mean standard error
					Comparative example 1	10	120	115	36
Example 1	9	257.1	96.2	32

Mu (. mu.) (product of example 1) -mu (. mu.) (product of comparative example 1)

Difference estimation value: -136.7

95% confidence interval for difference: (-239.4, -34.1)

T-test with difference 0 (and ≠): t-2.82, P-0.012, and 16 degrees of freedom.

Test example 5 Fulvine content test

FIG. 2 shows the results of testing the content of furfuryl acid in the products of comparative example 1 and example 1 (before modification in FIG. 2, the preparation method of comparative example 1, after modification, the preparation method of example 1, the modification stage 1, the sterilization treatment in the preparation method of example 1, and the modification stage 2, the protein stabilization treatment in the preparation method of example 1). As can be seen from FIG. 2, the mean level of the furfuryl acid content of the product of comparative example 1 is 116.80mg/100g of protein, and the mean level of the furfuryl acid content of the product of example 1 is 144.82mg/100g of protein. Therefore, the heat treatment strength can be effectively improved by increasing the protein stabilizing treatment, the furfuryl acid level of the UHT sterilized milk prepared is increased, but is still far lower than 190mg/100g of protein of the recovered milk, and the UHT sterilized milk meets the agricultural industry standard requirement.

According to the results provided by the test examples 1-5, the content of the furosine in the UHT sterilized milk product prepared by the invention is 150mg/100g protein, and the upper limit of the protease activity of the product is 140u/100ml 100-140u/100ml after the product is kept at 37 ℃ for 7 days, so that the product can be guaranteed to have a shelf life of 6 months.