CN100441099C - Method for inhibiting brown stain of low lactose milk and products thereof - Google Patents
Method for inhibiting brown stain of low lactose milk and products thereof Download PDFInfo
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Abstract
The present invention relates to a method for processing milk and a product obtained in the method, specifically to a method for inhibiting browning of low-lactose milk and a product thereof, which belongs to the field of dairy products and dairy processing. Lactase is added in milk at the temperature of 8 to 9 DEG C when the pH is from 6.6 to 6.8, wherein the enzyme consumption is from 0.5 to 0.75%, and the enzymolysis time is from 8 to 14 hours; the sterilization process is carried out at the temperature of 138 to 140 DEG C for 4.5 to 3.5 s; simultaneously, an inhibitor A or B is added in the sterilization process. The processed milk has the characteristics of low lactose, and clean and fresh flavor; simultaneously, the browning generated from sugar decomposition is inhibited.
Description
[technical field]
The present invention relates to a kind of processing method of milk and the product that obtains with the method, specifically, relate to a kind of method that suppresses the low-lactose milk brown stain, and the no brown stain milk that obtains with the method.Belong to the field that dairy products and Dairy Processing are handled.
[background technology]
Breast is the optimal natural food that various mammals feed its young baby, is rich in mineral matter and multivitamins such as nutritional labelings such as high-quality protein, butterfat, lactose and calcium, phosphorus, potassium.In developed country, breast and dairy products have become the important composition content of people's diet; Clearly emphasized " one day one glass of milk (250ml) of a people " in " the Chinese residents dietary guidelines " of the new revision of China, and WHO also classifies dairy products consumption figure per capita as the leading indicator of a national people's living standard of measurement.This shows the important function that cow's milk has in people's diet.
Although cow's milk has good nutritive value, in China, the year pre-capita consumption quantity not sufficient 10Kg of dairy products in 2000 is well below world's year dairy products consumption figure (100Kg) per capita.Except the development of China dairy industry and level of processing relatively lagged behind, lactose intolerance was also to a certain degree limiting the popularization of dairy products in China.
Lactose in Milk content is about 4.8% (Gu Ruixia, 2000), accounts for more than 99% of milk total reducing sugar.Under the normal physiological conditions, lactose after the lactase effect, is hydrolyzed to glucose and galactolipin and just can be absorbed by the body in small intestine.Investigation shows, the whole world (particularly Asia and Africa country) has approximately in 70% human body and lack lactase, take in cow's milk among these crowds after, bad reactions such as diarrhoea, ventosity appear, i.e. lactose intolerance (Fox etal., 1992).Therefore, in the process of Dairy Processing, utilize the low-lactose milk of lactase degraded lactose production not only can provide the high-quality glycogen, concerning the crowd who suffers from lactose intolerance, also increase their milk intake greatly to people.
Chinese patent CN1258452A discloses a kind of method with producing low-lactose milk with solid thermophilic bacteria lactase, wherein, temperature parameter and bacterial classification using method with the producing low-lactose milk with solid thermophilic bacteria lactase method are disclosed, but in the process of sterilization, can be owing to the carbonyl that decomposes in the reduced sugar that obtains combines with epsilon-amino in the lysine, Maillard reaction takes place, and causes low-lactose milk to produce non-enzymatic browning.Can't obtain qualified product.
Because in process, lactose is broken down into glucose and galactolipin at low-lactose milk, increased sugariness on the one hand, give good mouthfeel of low-lactose milk and local flavor; On the other hand, the carbonyl in a large amount of reduced sugars combines with epsilon-amino in the lysine, and Maillard reaction takes place, and causes low-lactose milk to produce non-enzymatic browning.
Maillard reaction is under the high temperature heating condition, between protein and the sugar carbonyl-ammonia react takes place, and it is the key factor that breast and dairy products produce brown stain.The first step of Maillard reaction is amino and carbonyl reacts with the open chain form, generates Schiff ' s alkali, is thereafter the Amadori molecular rearrangement reaction, generate N-and replace-1 amino-1-deoxidation-2-ketose, this material is colourless, does not absorb near the light in ultra-violet (UV) band, along with the carrying out of reaction, this material enol turns to 1,2-monoene amino alcohol or 2,3-alkene triol, the former finally forms 5 hydroxymethyl furfural (5-Hydroxymethylfurfural, 5-HMF) (Guo Benheng, 2001).The accumulation of 5-HMF and brown stain have very big correlation (Ferrer et al., 2000), because 5-HMF can break to form α-dicarbonyl compound, melanoidin (the Morale et al. that this carbonyls and amine reaction produce, 1992), be the key factor that causes breast and dairy products brown stain.Therefore, can produce the degree that reduces the product brown stain by control 5-HMF.
The present invention utilizes the lactase hydrolysis to produce low-lactose milk, utilize HPLC method (Morales et al., 1992) measure the content of the main intermediate product 5-HMF of Maillard reaction, and take this as a foundation and analyze different working conditions and of the influence of different inhibitor 5-HMF content in the low-lactose milk.In addition, the present invention also measures at the aberration of the low-lactose milk of gained under different sterilising conditions and the degree of hydrolysis condition, analyzes the relation between aberration and the 5-HMF content.
[summary of the invention]
The purpose of this invention is to provide a kind ofly provides a kind of method to handle milk, makes its characteristic with low lactose, the brown stain that is produced when suppressing to decompose sugar simultaneously, and also local flavor is clean and fresh;
Another object of the present invention provides a kind of low-lactose milk that does not have brown stain.
The technical solution adopted for the present invention to solve the technical problems is:
Get a certain amount of milk, be 6.6～6.8 at pH, under the condition of 8～9 ℃ of temperature, add lactase in milk, wherein enzyme dosage is 0.5 ‰～0.75 ‰ (weight portion), enzymolysis time 14～8 hours; , preferably use 0.5 ‰ (weight portion) enzyme dosage enzymolysis 14 hours, or 0.75 ‰ (weight portion) enzyme dosage enzymolysis 8 hours.
Can also carry out the high temperature enzymolysis, promptly in the time of 37～40 ℃, enzyme dosage is 0.5 ‰～0.75 ‰ (weight portion), 3～2 hours time, preferably under 37 ℃, with 0.5 ‰ (weight portion) enzyme dosage enzymolysis 3 hours, or 40 ℃ down with 0.75 ‰ (weight portion) enzyme amount enzymolysis 2 hours; Can reach and satisfy percent hydrolysis more than 70%, hydrolysis rate is fast;
In the sterilization process, operating parameter is selected as follows: at the 138-140 ℃ of 4.5-3.5s that sterilizes down;
In sterilization process, add inhibitor sodium sulfite or cysteine.
Consider cost and percent hydrolysis, in actual production, produce low-lactose milk, do not need lactose is all decomposed, when the percent hydrolysis of lactose in the low-lactose milk reaches 70%, just can solve the problem of lactose intolerance.Percent hydrolysis is when 70% left and right sides, and 5-HMF content is lower.Therefore, can reduce the generation of 5-HMF at the percent hydrolysis that satisfies control low-lactose milk under the situation of production requirement.
[description of drawings]
Fig. 1 utilizes lactose in the lactase degraded cow's milk to produce the process chart of no brown stain low-lactose milk;
The situation of change of percent hydrolysis when Fig. 2 is low temperature enzymolysis (8～10 ℃);
The situation of change of percent hydrolysis when Fig. 3 is high temperature enzymolysis (37～40 ℃);
Fig. 4 be the HPLC method collection of illustrative plates that detects 5-HMF go out the peak situation;
Fig. 5 is the linear relationship of 5-HMF content (C5-HMF) and peak area (Aera);
Fig. 6 is the influence of percent hydrolysis to 5-HMF content in the low-lactose milk;
Fig. 7 is the influence of sterilising temp to 5-HMF content;
Fig. 8 inhibitor is to the influence of 5-HMF content in the different sterilising temp low-lactose milks;
Fig. 9 inhibitor is to 5-HMF content influence in the different percent hydrolysis low-lactose milks;
Figure 10 represents to comprise minute surface reflex time 5-HMF content and aberration (Δ L
*, Δ a
*With Δ b
*) relation;
Figure 11 represents to get rid of minute surface reflex time 5-HMF content and aberration (Δ L
*, Δ a
*With Δ b
*) relation.
[specific embodiment]
Following examples are used to illustrate the present invention in conjunction with the accompanying drawings, but are not used for limiting the scope of the invention.
In the low-lactose milk production technology shown in Figure 1,5-HMF mainly results from sterilization phase, and the hot conditions in this stage is the principal element that causes Maillard reaction;
In Fig. 2, cryogenic conditions is produced low-lactose milk down, and enzyme dosage is 0.1 ‰ and 0.25 ‰ o'clock, and percent hydrolysis is lower at 4～16 hours; Enzyme dosage is 0.5 ‰ and 0.75 ‰, and percent hydrolysis rises very fast, reaches more than 70% at 14 hours and 8 hours respectively;
In Fig. 3, produce low-lactose milk under the hot conditions, enzyme dosage is 0.1 ‰ and 0.25 ‰ o'clock, percent hydrolysis is lower at 1～5 hour; Enzyme dosage is 0.5 ‰ and 0.75 ‰, and percent hydrolysis rises very fast, reaches more than 70% after 3 hours and 2 hours respectively;
As can be seen from Figure 4, retention time is when the 3.1min left and right sides, and the peak area at a peak, b peak, c peak increases along with sample introduction concentration and increases successively, and promptly a, b and c place go out the peak situation for 5-HMF through the HPLC analysis.
Concentration with sample is abscissa, and peak area is an ordinate, makes the calibration curve of 5-HMF, obtains the linear relationship of concentration and peak area, and the result as shown in Figure 5.5-HMF content is expressed as C5-HMF, and linear equation is Aera=14363C5-HMF+2.1617, and the correlation between the two reaches 99.89%.
After the HPLC method detects, obtain peak area through pretreated testing sample, then according to calibration curve shown in Figure 5, calculating can obtain the content of 5-HMF in the sample.
In the low-lactose milk production process, along with percent hydrolysis increases, content of reducing sugar raises.Under the situation of 139 ℃ of sterilization 4s, percent hydrolysis is for influence such as the Fig. 6 of 5-HMF content in the low-lactose milk of sterilization back.
As can be seen from Figure 6, along with percent hydrolysis raises, 5-HMF content increases in the low-lactose milk.The inventor finds, when the percent hydrolysis of lactose in the low-lactose milk reaches 70%, just can solve the problem of lactose intolerance.As shown in Figure 6, percent hydrolysis is when 70% left and right sides, and 5-HMF content is lower.Therefore, can reduce the generation of 5-HMF at the percent hydrolysis that satisfies control low-lactose milk under the situation of production requirement.
Produce in the process of low-lactose milk, will be after enzymolysis finishes to the enzymolysis liquid high-temperature process, reaching the enzyme that goes out, sterilization, thus the purpose that extends the shelf life.And the easiest generation Maillard reaction also is sterilization phase.Under the high-temperature sterilization condition, the reduced sugar that contains in the low-lactose milk and the amino acid residue of protein react, and have produced the intermediate product 5-HMF of Maillard reaction.Different sterilising temps and temperature retention time are to influence such as the Fig. 7 of 5-HMF content in the low-lactose milk.
As Fig. 7, sterilising temp and time are all influential to the content of 5-HMF.Sterilising temp is high more, and the 5-HMF content that low-lactose milk produces is also many; Sterilization time is long more, and 5-HMF content is high more.Producing long shelf-life during sterilized milk, 139 ℃, 4s or 135 ℃, the 15s of adopting carry out UHTS more in the actual production, and as can be seen from Figure 7, sterilising conditions is 139 ℃, during 4s, and the 5-HMF content of generation still less.
As can be seen from Figure 8, under all sterilising temps, even sterilization time is grown (15s), 5-HMF content all is lower than 5-HMF content in the low-lactose milk that does not add any inhibitor in the low-lactose milk behind the interpolation inhibitor.After adding inhibitor sodium sulfite or cysteine, it is less that the content of 5-HMF is subjected to the influence of sterilising temp, but cysteine suppresses the better effects if that 5-HMF produces.
It is 139 ℃ that the inventor has analyzed sterilising conditions, during 4s, add inhibitor to 5-HMF content influence in the different percent hydrolysis low-lactose milks, result such as Fig. 9.As Fig. 9, behind the interpolation inhibitor, 5-HMF content all is lower than the low-lactose milk that does not add any inhibitor in the low-lactose milk of different percent hydrolysis.Along with percent hydrolysis raises, the recruitment of 5-HMF is lower than the product that does not add inhibitor in the low-lactose milk behind the interpolation inhibitor, and under all percent hydrolysis conditions, cysteine suppresses the better effects if that 5-HMF produces.
As shown in figure 10, comprise under the situation of minute surface reflection brightness value Δ L
*Along with 5-HMF content raises and reduces, promptly the color of low-lactose milk raises with 5-HMF content and progressively deepens, and this change in color can perusal.5-HM content and Δ L
*Between have binomial relation, the same, 5-HMF content is expressed as C5-HMF, Δ L
*And the mathematical relationship between the C5-HMF is: Δ L
*=-0.004 (C5-HMF) 2-0.3154C5-HMF+0.1381, correlation reaches 99.44%.And red scale value Δ a
*With yellow value degree Δ b
*Raise along with the rising of 5-HMF content.Δ a
*And the mathematical relationship between the C5-HMF is expressed as Δ a
*=-0.0027 (C5-HMF) 2+0.2697C5-HMF-0.1581 correlation reaches 99.07%.Δ b
*And the mathematical relationship between the C5-HMF is expressed as Δ b
*=0.0036 (C5-HMF) 2+0.2369C5-HMF-0.5693, correlation is 94.91%.
As Figure 11, under the situation of getting rid of the minute surface reflection, 5-HMF content and aberration (Δ L
*, Δ a
*With Δ b
*) also there is the trend identical with comprising the minute surface reflex time.Brightness value Δ L
*Reduce with the rising of 5-HMF content, the mathematical relationship between the two is Δ L
*=-0.0058 (C5-HMF) 2-0.3129C5-HMF+0.1389, correlation reaches 99.58%.Red scale value Δ a
*With yellow value degree Δ b
*Raise along with the rising of 5-HMF content.Δ a
*And the mathematical relationship between the C5-HMF is expressed as Δ a
*=-0.0024 (C5-HMF) 2+0.2854C5-HMF-0.1671, correlation is 99.15%.Δ b
*And the mathematical relationship between the C5-HMF is expressed as Δ b
*=0.0063 (C5-HMF) 2+0.2371C5-HMF-0.6319, correlation is 95.56%.
From the above analysis, 5-HMF content and its aberration (Δ L in the low-lactose milk
*, Δ a
*With Δ b
*) exist binomial to concern.No matter in the testing process, whether the reflection of the minute surface of cuvette exists the brightness value Δ L of low-lactose milk
*Reduce red scale value Δ a with the rising of 5-HMF content
*With yellow value degree Δ b
*All raise with 5-HMF content.
For the relation of 5-HMF content and aberration in the clear and definite low-lactose milk, the inventor has detected under the situation of different 5-HMF content, aberration (Δ L
*, Δ a
*With Δ b
*) situation of change, analyzed the mathematical relationship between 5-HMF content and the aberration simultaneously.Figure 10 represents to comprise minute surface reflex time 5-HMF content and aberration (Δ L
*, Δ a
*With Δ b
*) relation, Figure 11 represents to get rid of minute surface reflex time 5-HMF content and aberration (Δ L
*, Δ a
*With Δ b
*) relation.
Embodiment 1
The HPLC method detects 5-HMF
Among the present invention, adopt the HPLC method to measure Ruzhong 5-HMF content.Get the 5-HMF standard items of three kinds of variable concentrations (1.1088 μ mol/ml, 3.3264 μ mol/ml, 6.6528 μ mol/ml), analyze with HPLC, be determined at the absorption at 280nm place, sample size is 20 μ l.
The relation of 5-HMF content and aberration in the low-lactose milk
The inventor has analyzed the relation of 5-HMF content and aberration in the low-lactose milk, verifies to use and measures the feasibility that 5-HMF content is monitored the low-lactose milk brown stain.
Utilize lactase hydrolysis cow's milk, degree of hydrolysis be respectively 52.1%, 68.7%, 69.6% and 76.1% o'clock the sampling, and the sample of the different percent hydrolysis of gained carried out two kinds of processing: 85 ℃ of sterilization 15min, 121 ℃ of sterilization 10min measure the 5-HMF content and aberration (the Δ L of each sample then
*, Δ a
*With Δ b
*).The detection of aberration is a standard sample with the raw material milk of corresponding sterilising conditions respectively under two kinds of sterilising conditions.Raw material milk through 85 ℃ the sterilization 15min after, L
*=76.81, a
*=-2.11, b
*=4.36; Raw material milk through 121 ℃ the sterilization 10min after, L
*=73.02, a
*=1.0, b
*=10.10.Gained hangs down 5-HMF content and its aberration result such as table 1 in the milk sugar specimen behind enzymolysis:
5-HMF and value of chromatism in the different degree of hydrolysis low-lactose milks under two kinds of sterilising conditions of table 1
As table 1, under high-temperature sterilization (the 121 ℃ of sterilization 10min) condition, the 5-HMF content of low-lactose milk is higher than low temperature sterilization (85 ℃ of sterilization 15min) far away, simultaneously, and brightness value Δ L
*Value during well below low temperature sterilization.As seen, under the identical situation of percent hydrolysis, the color of low-lactose milk product is darker during high-temperature sterilization.
Adopt and use the same method, analyzed under the different sterilising conditions, percent hydrolysis is 5-HMF content and an aberration in 68.1% the low-lactose milk, as table 2.
5-HMF content and aberration in the low-lactose milk under the different sterilising conditions of table 2
As can be known from Table 2, sterilising temp raises, and 5-HMF content raises in the low-lactose milk, and the low-lactose milk product colour is deepened.
From table 1 and table 2 as can be seen, under the different treatment conditions, great changes have taken place for the content of 5-HMF in the low-lactose milk, and simultaneously, its value of chromatism also changes along with the variation of 5-HMF content.
Key instrument: island Tianjin-high performance liquid chromatograph, SPD-10AVP/10AVVP ultraviolet-visible detector, DGU-12A automatic deaerating device, U.S. Rite SP62 spectrophotometer
Reagent: lactase (EC 3.2.1.23), 5 hydroxymethyl furfural (5-HMF, Sigma), methyl alcohol (RomilChemicals, chromatographically pure), it is pure that crystallization sodium acetate, acetate, trichloroacetic acid, oxalic acid, inhibitor sodium sulfite and cysteine are analysis, distilled water.
The mensuration of lactose hydrolysis ratio
Lactose hydrolysis ratio adopts enzyme to urge method, utilizes kit to measure.
Principle: a part lactose produces a part glucose and a part galactolipin in the cow's milk after the lactase hydrolysis, and therefore, available glucose oxidase-peroxidase method detects the content of glucose in the cow's milk single-mindedly, thus the percent hydrolysis of lactose as can be known.Glucose generates gluconic acid and hydrogen peroxide through glucose oxidase, hydrogen peroxide further discharges nascent oxygen behind the peroxide oxydasis, this oxygen is under the condition that phenol exists, can make the amino antipyrine of colourless 4-(reduced form) be oxidized to red quinonoid compound (oxidized form), this material has maximum light absorption value at the 505nm place, and the depth of color is directly proportional with glucose content in the sample.Reaction condition is 37 ℃, 15min, and course of reaction can be represented by the formula:
Glucose content and lactose hydrolysis ratio are calculated as follows in the sample:
Glucose content in the sample (g/L)=(measuring pipe absorbance/standard pipe absorbance) * normal concentration
Lactose hydrolysis ratio (%)=(glucose content in 2 * sample)/lactose content * 100%
Embodiment 4
Determining of enzymatic hydrolysis condition
Utilize lactase (EC 3.2.1.23) hydrolyzes lactose, produce low-lactose milk.The simulation working condition adopts low temperature enzymolysis (8～10 ℃) and high temperature (37～40 ℃) enzymolysis, pH6.6～6.8, and enzyme dosage is all established 4 concentration: 0.1 ‰, 0.25 ‰, 0.5 ‰, 0.75 ‰.Enzyme dosage and enzymolysis time are determined in the variation of 4～16 hours percent hydrolysis of monitoring low temperature enzymolysis process, and the situation of change of 1～5 hour percent hydrolysis of high temperature enzymolysis process then.
The 5-HMF Determination on content
Utilize the HPLC method to measure 5-HMF content (Morales et al., 1992).
Chromatographic condition is as follows:
Chromatographic column: Resolve C18 chromatographic column (150mm * 4.0mm, Dalian Yi Lite scientific instrument Co., Ltd)
Phase flows: 0.1M pH3.8 sodium-acetate buffer: methyl alcohol=92: 10
Detect wavelength: UV-detector detects, wavelength 280nm
Sample size: 20 μ l
The preparation of standard liquid: with the dissolving of 0.056g 5-HMF standard items, constant volume is mixed with stoste to 200ml, gets 0.1ml, 0.3ml, 0.6ml stoste more respectively earlier, adds 5ml 0.15M oxalic acid, 3ml 40%TCA and 10ml4%TCA, and constant volume is to 25ml then.
Sample pretreating method is with reference to Ferrer (2000), and idiographic flow is as follows: add the 5ml0.15M oxalic acid solution in 15ml milk, heat 25min behind the mixing in boiling water.Thing to be mixed is cooled to room temperature, adds 3ml40%TCA again, fully vibration, and it is centrifugal that (2000 * g 15min), collects supernatant.Add 10ml 4%TCA again in centrifugation, centrifugal behind the mixing (2000 * g 15min), collects supernatant.Merge two times centrifugal supernatant, measure volume, by micro-filtration membrane (0.45 μ m), gained filtrate is detected with HPLC then.
Embodiment 5
Aberration detects
Utilize above-mentioned lactase to prepare low-lactose milk, enzyme dosage is 0.5 ‰.
The aberration of gained low-lactose milk sample U.S. Rite SP 62 spectrophotometric determinations.Step: spectrophotometer is placed the difference display mode, calibrate with white standard then; Sample standard is injected colorimetric pool, and colorimetric pool places on the special-purpose colorimetric shelf, the aberration of first bioassay standard sample, and then with the aberration of identical method working sample.With CIE L
*a
*b
*Be the tolerance pattern (Bertelli et al., 1996) of sample aberration, L
*Be brightness value, a
*Red scale value, b
*Be yellow value degree, L
*, a
*And b
*Variation be calculated as follows:
Δ L
*=L
*-L
*0 (L
*Be sample brightness value, L
*0 is the standard sample brightness value)
Δ a
*=a
*-a
*0 (a
*Be sample red scale value, a
*0 is the standard sample red scale value)
Δ b
*=b
*-b
*0 (b
*Be sample yellow value degree, b
*0 is the standard sample yellow value degree)
Among the gained result, if Δ L
*For just, the interpret sample brightness value is than standard sample height, and is of light color; If Δ L
*For negative, the interpret sample brightness value is lower than standard sample, and color is dark.
Embodiment 6
Get a certain amount of milk, be 6.6 at pH, under the condition of 9 ℃ of temperature, add lactase in milk, wherein enzyme dosage is 0.5 ‰ (weight portions), enzymolysis time 14 hours; In the sterilization process, operating parameter is selected as follows: at 139 ℃ of 4s that sterilize down.
Embodiment 7
Get a certain amount of milk, be 6.8 at pH, under the condition of 9 ℃ of temperature, add lactase in milk, wherein enzyme dosage is 0.75 ‰ (weight portion), enzymolysis time 8 hours; In the sterilization process, operating parameter is selected as follows: at 138 ℃ of 4.5s that sterilize down.
Embodiment 8
A kind of method that suppresses the low-lactose milk brown stain is characterized in that: get a certain amount of milk, be 6.8 at pH, under the condition of 8 ℃ of temperature, add lactase in milk, wherein enzyme dosage is 0.75 ‰ (weight portion), enzymolysis time 8 hours; In the sterilization process, operating parameter is selected as follows: at 140 ℃ of 4.5s that sterilize down.
Embodiment 9
A kind of method that suppresses the low-lactose milk brown stain is characterized in that: get a certain amount of milk, be 6.6 at pH, under the condition of 37 ℃ of temperature, add lactase in milk, wherein enzyme dosage is 0.75 ‰ (weight portion), enzymolysis time 2 hours; In the sterilization process, operating parameter is selected as follows: at 139 ℃ of 4s that sterilize down.
A kind of method that suppresses the low-lactose milk brown stain is characterized in that: get a certain amount of milk, be 6.6 at pH, under the condition of 40 ℃ of temperature, add lactase in milk, wherein enzyme dosage is 0.5 ‰ (weight portions), enzymolysis time 14 hours; In the sterilization process, operating parameter is selected as follows: at 139 ℃ of 4s that sterilize down.
Embodiment 11
A kind of method that suppresses the low-lactose milk brown stain is characterized in that: get a certain amount of milk, be 6.8 at pH, under the condition of 40 ℃ of temperature, add lactase in milk, wherein enzyme dosage is 0.5 ‰ (weight portions), enzymolysis time 14 hours; In the sterilization process, operating parameter is selected as follows: at 139 ℃ of 4s that sterilize down.Effect of the present invention is as follows:
Through the selection of the present invention through parameter, the time of enzymolysis and parameter, sterilising temp and percent hydrolysis, selection of inhibitors, after a large amount of experiment of process, the inventor has obtained optimized parameter, make to prepare in the process of low-lactose milk, suppress brown stain well, and can get a desired effect.
Claims (6)
1. method that suppresses the low-lactose milk brown stain, it is characterized in that: get a certain amount of milk, be 6.6～6.8 at pH, under the condition of 8～9 ℃ of temperature, in milk, add lactase, wherein enzyme dosage is 0.5 ‰～0.7 ‰ (weight portions), enzymolysis time 14～8 hours; In the sterilization process, operating parameter is selected as follows: at the 138-140 ℃ of 4.5-3.5s that sterilizes down, wherein, add inhibitor sodium sulfite or cysteine in sterilization process.
2. the method for inhibition low-lactose milk as claimed in claim 1 brown stain, when wherein said enzymatic hydrolysis condition was 37～40 ℃, the consumption of lactase was 0.5 ‰～0.7 ‰ (weight portions), enzymolysis time 3～2 hours.
3. the method for inhibition low-lactose milk as claimed in claim 2 brown stain, wherein said enzymatic hydrolysis condition is 40 ℃, the consumption of lactase is 0.7 ‰ (weight portions), enzymolysis time 2 hours.
4. the method for inhibition low-lactose milk as claimed in claim 2 brown stain, when wherein said enzymatic hydrolysis condition was 37 ℃, the consumption of lactase was 0.5 ‰ (weight portions), enzymolysis time 3 hours.
5. as the method for claim 1 or 2 said inhibition low-lactose milk brown stains, wherein, 4s sterilize under 139 ℃.
6. a no brown stain low-lactose milk is characterized in that producing with any one described method among the claim 1-5.
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| CN101228904B (en) * | 2008-02-26 | 2012-03-21 | 内蒙古蒙牛乳业（集团）股份有限公司 | Low-lactose milk and preparation method thereof |
| JP5621224B2 (en) * | 2009-08-06 | 2014-11-12 | 東洋製罐株式会社 | Method for producing containerized milk |
| AP3823A (en) * | 2010-12-10 | 2016-09-30 | Arla Foods Amba | Lactose-reduced milk-related product, and a process and milk processing plant for its manufacture |
| CN103891885A (en) * | 2012-12-25 | 2014-07-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | Browning process of dairy product |
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Non-Patent Citations (6)
| Title |
|---|
| Antiradical Efficiency of Malllard Reaction Mixtures in aHydrophilic Media. Francisco J. Morales, Maj-Britt Babbel.J.Agric.Food Chem.,Vol.50 . 2002 |
| Antiradical Efficiency of Malllard Reaction Mixtures in aHydrophilic Media. Francisco J. Morales, Maj-Britt Babbel.J.Agric.Food Chem.,Vol.50. 2002 * |
| 低乳糖牛乳的研制. 龚广予，李明.食品工业，第1期. 2000 |
| 低乳糖牛乳的研制. 龚广予，李明. 食品工业，第1期. 2000 * |
| 超高温低乳糖牛奶的研制. 丁裕海，冯立科.中国乳品工业，第30卷第5期. 2002 |
| 超高温低乳糖牛奶的研制. 丁裕海，冯立科. 中国乳品工业，第30卷第5期. 2002 * |
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