CN113758904A - Method for detecting stability of dairy product - Google Patents
Method for detecting stability of dairy product Download PDFInfo
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- 235000013365 dairy product Nutrition 0.000 title claims abstract description 161
- 238000000034 method Methods 0.000 title claims abstract description 69
- 238000012360 testing method Methods 0.000 claims abstract description 85
- 235000013336 milk Nutrition 0.000 claims description 21
- 239000008267 milk Substances 0.000 claims description 21
- 210000004080 milk Anatomy 0.000 claims description 21
- 230000008859 change Effects 0.000 claims description 4
- 235000015140 cultured milk Nutrition 0.000 claims description 3
- 235000020124 milk-based beverage Nutrition 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 claims description 2
- 235000020201 recombined milk Nutrition 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 239000000047 product Substances 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 30
- 235000013618 yogurt Nutrition 0.000 description 16
- 238000005119 centrifugation Methods 0.000 description 15
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- 238000004364 calculation method Methods 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000003921 particle size analysis Methods 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 230000009471 action Effects 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 235000020251 goat milk Nutrition 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
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- 238000007781 pre-processing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/59—Transmissivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/10—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material
- G01N11/14—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by moving a body within the material by using rotary bodies, e.g. vane
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Abstract
The invention belongs to the technical field of quality detection of dairy products, and particularly provides a method for detecting the stability of a dairy product, which comprises the following steps of (1) determining the viscosity eta of the dairy product to be detected; (2) a pretreatment step; (3) the method for testing the stability of the dairy product has the advantages of high accuracy, high precision, good repeatability, simple and quick detection method, wide detection range and suitability for testing the dairy product with the viscosity range lower than 15000 cp.
Description
Technical Field
The invention belongs to the technical field of quality detection of dairy products, and particularly relates to a method for detecting the stability of a dairy product.
Background
The dairy product refers to various foods prepared by using cow milk or goat milk and processed products thereof as main raw materials, adding or not adding appropriate amount of vitamins, minerals and other auxiliary materials and using conditions required by laws, regulations and standards, and is also called dairy products. Because the dairy product contains certain protein and fat, sometimes a thickening agent or colloid is added, instability problems such as water separation, precipitation, fat floating, flocculation and the like can occur within the shelf life of 6-12 months after the product is sterilized at high temperature. Therefore, the establishment of the stability detection method of the dairy product has important significance for inspecting the quality of the dairy product.
At present, the traditional method for judging the stability of the milk system mainly comprises an observation method, a particle size analysis method, a centrifugal precipitation method and the like. The methods have more problems in practical application, for example, the method has limitation when the stability of the shelf life of the dairy product is judged by using an observation method, the observation result is greatly influenced by subjectivity, and the method is more suitable for products with short shelf life; although the particle size analysis method can indirectly reflect the stability of the product by measuring the particle size of the product, the particle size analysis method cannot reflect the movement track of particles in a product system, and has limitations; the centrifugation method adopts a centrifugation mode, is simple and easy to operate, but has poor repeatability, larger error of test results and is not suitable for products with higher viscosity, so the method has no universal applicability.
The Wangchengxi and the like adopt a LUMi-Sizer stability analyzer to investigate the stability influence of a thickening agent on oat beverage, for the oat beverage with high viscosity, the result obtained by the method is completely inconsistent with the result obtained by an observation method, the method cannot be used independently, a more accurate stability result can be obtained only by combining a Turbiscan stability tester, and the problems of low precision and poor repeatability also exist, so that the test needs two sets of instruments, the test time is long, the cost is high, and the application range is narrow. The influence of the thickening agent on the stability of the oat beverage is researched by applying a rapid stability analysis method [ J ]. the food and fermentation industry, 2018,44(3)253 and 259.
Disclosure of Invention
The invention aims to overcome the defects of low accuracy and precision, poor repeatability, long testing time and narrow application range of the detection method in the prior art on the dairy product with higher viscosity, and further provides the detection method for the stability of the dairy product, which is rapid and accurate, high in precision, good in repeatability and wide in detection range.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for detecting the stability of dairy products comprises the following steps:
(1) measuring the viscosity of the dairy product to be measured;
(2) a pretreatment step: when eta is more than 2000 and less than 10000cp, centrifuging the dairy product to be detected for 0.5-3min at 4000rpm of 2500-; when eta is more than or equal to 10000 and less than 15000cp, centrifuging the dairy product to be detected for 0.5-3min at 3500-;
(3) instability index determination step: and (3) measuring the light transmittance change of the dairy product to be measured with eta less than or equal to 2000cp, the dairy product to be measured with eta less than or equal to 2000cp after the pretreatment in the step (2) or the dairy product to be measured with eta less than or equal to 10000cp after the pretreatment in the step (2) at the rotation speed of 1000-4000rpm by adopting a stability analyzer through infrared scanning to obtain the instability index.
Further, in the step (2), the pretreatment step of the dairy product to be detected with the eta of more than or equal to 10000 and less than 15000cp is to centrifuge at 4000rpm for 0.5-2min, then centrifuge at 3500rpm for 0.5-1min, centrifuge at 3000rpm for 0.5-1min and centrifuge at 2500rpm for 0.5-1 min.
Further, in the step (2), the pretreatment step of the dairy product to be detected with the eta of more than 2000 and less than 10000cp is to firstly centrifuge for 0.5-2min at 4000rpm and then centrifuge for 0.5-1min at 3500 rpm.
In the step (3), the testing temperature is 20-35 ℃, and the scanning is performed once every 5-20s for 100-.
Further, for the dairy product to be tested with eta less than or equal to 2000cp, the test conditions in the step (3) are as follows: the rotating speed is 3000 plus 4000 rpm; the testing rotating speed of the dairy product to be tested with the viscosity of 2000< eta <10000cp is 2000-4000 rpm; the testing rotation speed of the dairy product to be tested with the viscosity of 10000 ≤ eta <15000cp is 1000-3000 rpm.
Further, for the dairy product to be tested with eta less than or equal to 2000cp, the test conditions in the step (3) are as follows: the rotating speed is 3500rpm, the testing temperature is 25 ℃, the scanning is carried out once every 15s for 150 times, and the light intensity factor is 1.0.
Further, for the dairy product to be tested with the viscosity of 2000< η <10000cp, the test conditions in the step (3) are as follows: the rotating speed is 3000rpm, the testing temperature is 25 ℃, the scanning is carried out once every 10s for 180 times, and the light intensity factor is 1.0.
Further, for the dairy product to be tested with the viscosity of 10000 ≤ η <15000cp, the test conditions in the step (3) are as follows: the rotating speed is 2000rpm, the testing temperature is 25 ℃, the scanning is carried out once every 8s, the total scanning is 220 times, and the light intensity factor is 1.0.
Further, the stability analyzer is a LUMi-Sizer stability analyzer and/or a LUMiFuge stability analyzer.
Further, the dairy product is at least one of milk, prepared milk, beverage and fermented milk.
The accuracy refers to the difference between the measured value and the actual value, and the higher the accuracy, the smaller the difference between the measured value and the actual value. The degree of dispersion of each data from the mean is generally described by the standard deviation, expressed as SD, with greater values being less stable and less accurate.
Precision refers to the proximity between the measured values of multiple parallel measurements, and the higher the precision, the closer the measured values of multiple parallel measurements are. The precision of the analytical test results is often expressed in terms of RSD. When performing statistical analysis of data, if the RSD is greater than 15%, the data should be rejected considering that it may not be normal.
The technical scheme of the invention has the following advantages:
(1) the method for detecting the stability of the dairy product comprises the steps of measuring the viscosity of the dairy product to be detected, preprocessing and measuring the instability index, wherein the dairy product to be detected with the viscosity of 2000< eta <10000cp is centrifuged for 0.5-3min at 2500-; centrifuging the to-be-detected dairy product with eta <15000cp being more than or equal to 10000 for 0.5-3min at 3500-; the instability index is measured under the optical scanning action of 1000-4000rpm after the pretreatment step, the accuracy, precision and repeatability of the method for measuring the dairy product with higher viscosity can be obviously improved by adding the pretreatment step, and the method is simple and quick, is suitable for measuring various dairy products with the viscosity range lower than 15000cp, and has wide detection range.
(2) The method for detecting the stability of the dairy product comprises the steps of firstly measuring the viscosity of the dairy product to be detected, innovatively selecting different test conditions for the dairy product to be detected with different viscosities, wherein the instability index of the dairy product to be detected with eta less than or equal to 2000cp is tested under the conditions that the rotating speed is 3000-4000rpm and the temperature is 20-35 ℃, and the instability index of the dairy product to be detected with the viscosity being 2000< eta <10000cp is tested under the conditions that the rotating speed is 2000-4000rpm and the temperature is 20-35 ℃; for the dairy product to be tested with the eta of more than or equal to 10000 and less than 15000cp, the instability index is tested under the conditions that the rotating speed is 1000-3000rpm and the temperature is 20-35 ℃, the samples to be tested with different viscosities are distinguished and determined, three sets of test methods are established, and the accuracy, the precision and the repeatability of the test methods are further improved.
(3) According to the method for detecting the stability of the dairy product, the dairy product to be detected with the eta of more than or equal to 10000 and less than 15000cp is subjected to the pretreatment step of centrifuging for 0.5-2min at 4000rpm, then sequentially centrifuging for 0.5min at 3500rpm, centrifuging for 0.5min at 3000rpm, and analyzing for 0.5min at 2500rpm, so that the accuracy, precision and repeatability of the test method can be further improved.
(4) Experiments show that for the dairy product to be tested with eta less than or equal to 2000cp, the test method obtained by controlling the rotating speed to be 3500rpm, the test temperature to be 25 ℃, scanning every 15s for 150 times and the light intensity factor to be 1.0 is more accurate and reliable; for the dairy product to be tested with eta of 2000< 10000cp, the test method is more accurate and reliable by controlling the test conditions in the step (3) to be 3000rpm, 25 ℃ of test temperature, scanning once every 10s and scanning 180 times in total, wherein the light intensity factor is 1.0; and (3) controlling the test conditions in the step (3) to be that the 10000 is more than or equal to eta less than 15000 cp: the rotating speed is 2000rpm, the testing temperature is 25 ℃, the scanning is carried out once every 8s, the scanning is carried out for 220 times in total, and the testing method obtained by the light intensity factor of 1.0 is more accurate and reliable.
(5) According to the method for detecting the stability of the dairy product, the LUMi-Sizer stability analyzer is adopted, a dynamic stability analysis method is utilized, the theory that the particle migration rate is in direct proportion to centrifugal force in the Stokes law and the theory that the response value of particles to light intensity in the migration process in the Lambert-beer law are in direct proportion are combined, the migration change of the particles is reflected through the change of the light intensity, the smaller the migration rate of the product particles is, the more stable the product is; the smaller the light intensity variation of the product, the more stable the product. The dairy products with excessive stability indexes have serious phenomena of fat floating, bleeding and precipitation, which not only affect the taste of the products but also are not beneficial to the storage of the products in terms of the quality of the products.
(6) According to the method for detecting the stability of the dairy product, firstly, the centrifugal rotating speed which is the same as that of a centrifugal method is selected, so that errors caused by different test conditions can be eliminated; secondly, the invention creatively adds a sample pretreatment link, which not only can ensure the uniform dispersion of the sample, but also can improve the stability of the test data; thirdly, the instability index is calculated by an instrument automatically without manual calculation, so that the calculation time is saved while errors caused by manual operation are eliminated; fourthly, the method is simple to operate, the required sample amount is small (2g), the loading is simple and quick, the centrifugal precipitation method or the centrifugal water loss method has a plurality of weighing links including the weighing of a centrifuge tube, a sample, supernatant or precipitation amount, more errors can be brought virtually, and the accuracy and precision of the test method are reduced.
(7) The maximum acceptable lability index of a dairy product will vary with the product and its intended use, and typically the maximum acceptable lability index of a dairy product is between 0.75 and 0.99. When 0.75 is selected as the maximum acceptable instability index, the instability index of the tested dairy product is less than or equal to 0.75, which indicates that the dairy product has good stability, and the instability index of the tested dairy product is greater than 0.75, which indicates that the dairy product has poor stability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIGS. 1-3 are test profiles of example 1;
FIGS. 4-6 are test profiles of example 2;
FIGS. 7-9 are test profiles of example 3;
FIGS. 10-12 are test profiles for example 4;
FIGS. 13-15 are test profiles of example 5;
FIGS. 16-18 are test profiles of example 6;
FIGS. 19-21 are test profiles of example 7;
FIGS. 22-24 are test profiles of example 8;
FIGS. 25-27 are test maps for example 9;
FIGS. 28-30 are test profiles of example 10;
FIGS. 31-33 are test profiles of example 11;
FIGS. 34-36 are test maps for example 12;
FIGS. 37-39 are test profiles of example 13;
40-42 are test maps for example 14;
FIGS. 43-45 are test profiles of example 15.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
1. Experimental apparatus and consumables:
the device comprises a BROOKFIELD (American) viscometer DV2T LV, a rotor with the model number of ULA, LV and T-A-T-F rotors, a LUMiSizer X65 (Germany) stability analyzer, a 2mm PC sample tube, a sample needle, a sample cap, a plurality of disposable syringes, a pair of scissors, a centrifuge (Allegra X-15R, American), a dropper, a plurality of 50ml centrifuge tubes, an analytical balance (with the precision of 0.001mg), a plurality of large weighing spoons and 12 glass rods.
2. Experimental samples:
milk, milk drinks, fermented milk, modified powdered yogurt, drinking yogurt, and stirred yogurt are commercially available.
Example 1 Low viscosity sample
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the commercial milk as the milk product to be measured, measuring the viscosity of the milk by using a viscometer and a rotor with the number ULA, repeating the measurement for three times, and taking an average value, wherein the viscosity of the commercial milk is 1.89 cp.
(2) 2.0g of uniformly mixed and bubble-free milk is loaded into a 2-mm PC sample tube, an LUMisizer X65 stability analyzer is adopted, the set rotating speed is 3000rpm, the scanning time interval is 15s, the total scanning frequency is 150 times, the testing temperature is 25 ℃, the light intensity factor is 1.0, optical analysis is carried out, each sample is repeatedly measured for three times, the instability index of the product is respectively read, and the repeatability, the accuracy and the precision are calculated, wherein the results are shown in Table 1.
Example 2 Low viscosity samples
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) the same batch of milk as in example 1 was taken as the dairy product to be tested.
(2) 2.0g of uniformly mixed and bubble-free milk is loaded into a 2-mm PC sample tube, a LUMiSizer X65 stability analyzer is adopted, the set rotating speed is 3500rpm, the scanning time interval is 15s, the total scanning frequency is 150 times, the testing temperature is 25 ℃, the light intensity factor is 1.0, the test is carried out, each sample is repeatedly measured for three times, the instability index of the product is respectively read, and the repeatability, the accuracy and the precision are calculated, and the results are shown in Table 1.
Example 3 Low viscosity samples
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) the same batch of milk as in example 1 was taken as the dairy product to be tested.
(2) 2.0g of uniformly mixed and bubble-free milk is loaded into a 2-mm PC sample tube, a LUMiSizer X65 stability analyzer is adopted, the set rotating speed is 4000rpm, the scanning time interval is 15s, the total scanning frequency is 150 times, the testing temperature is 25 ℃, the light intensity factor is 1.0 for determination, each sample is repeatedly determined for three times, the instability index of the product is respectively read, and the calculation repeatability, the accuracy and the precision are shown in Table 1.
Viscosity samples from example 4
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) and taking the commercial drinking yoghurt as the dairy product to be measured, repeatedly measuring for three times by adopting a viscometer and a T-B rotor, and taking an average value to measure the viscosity of the drinking yoghurt to be 7988.33 cp.
(2) A pretreatment step: taking 2.0g of the uniformly mixed and bubble-free dairy product to be detected, loading the dairy product to be detected into a 2mm PC sample tube, carrying out multiple pretreatment by adopting a fast and slow centrifugation mode, firstly centrifuging for 1min at 4000rpm, then centrifuging for 0.5min at 3500rpm, centrifuging for 0.5min at 3000rpm, and centrifuging for 0.5min at 2500 rpm.
(3) Taking the centrifuged dairy product to be tested, adopting a LUMiSizer X65 stability analyzer, setting the rotating speed to be 2000rpm, the scanning time interval to be 10s, the total scanning times to be 180 times, the testing temperature to be 25 ℃, the light intensity factor to be 1.0, carrying out continuous optical analysis, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 1.
Viscosity samples from example 5
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) the same batch of drinking yoghurt of example 4 was taken as the dairy product to be tested.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and the pretreatment is carried out for a plurality of times by adopting a fast and slow centrifugation mode, and the dairy product is firstly centrifuged for 1min at 4000rpm and then centrifuged for 0.5min at 3500 rpm.
(3) Taking the centrifuged dairy product to be tested, adopting a LUMiSizer X65 stability analyzer, setting the rotating speed to be 3000rpm, the scanning time interval to be 10s, the total scanning times to be 180 times, the testing temperature to be 25 ℃, and the light intensity factor to be 1.0 to perform continuous optical analysis, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 1.
Viscosity samples from example 6
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) the same batch of drinking yoghurt of example 4 was taken as the dairy product to be tested.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is loaded into a 2mm PC sample tube and is firstly centrifuged for 1min at 4000 rpm.
(3) Taking the centrifuged dairy product to be tested, adopting a LUMiSizer X65 stability analyzer, setting the rotating speed at 4000rpm, the scanning time interval at 10s, the total scanning times at 180 times, the testing temperature at 25 ℃, and the light intensity factor at 1.0 to perform continuous optical analysis, repeatedly measuring each sample for three times, respectively reading the instability index, the calculation repeatability, the accuracy and the precision of the product, and obtaining the result shown in Table 1.
Example 7 high viscosity samples
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the commercially available stirred yogurt as the dairy product to be measured, repeatedly measuring for three times by using a viscometer and a rotor with a number T-C, and taking an average value to measure the viscosity of the stirred yogurt to be 12081 cp.
(2) A pretreatment step: taking 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles, loading the dairy product to be detected into a 2mm PC sample tube, carrying out multiple pretreatment by adopting a fast and slow centrifugation mode, centrifuging for 1min at 4000rpm, sequentially centrifuging for 0.5min at 3500rpm, centrifuging for 0.5min at 3000rpm, centrifuging for 0.5min at 2500rpm, centrifuging for 0.5min at 2000rpm, and centrifuging for 0.5min at 1500 rpm.
(3) Taking the centrifuged dairy product to be tested, setting the rotating speed to be 1000rpm, the scanning time interval to be 8s, the total scanning times to be 220 times, the testing temperature to be 25 ℃, the light intensity factor to be 1.0 by adopting a LUMiSizer X65 stability analyzer, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 1.
Example 8 high viscosity samples
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the stirred yoghurt of the same batch in the example 7 as the dairy product to be detected.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and is subjected to multiple times of pretreatment by adopting a fast and slow centrifugation mode, wherein the dairy product is firstly centrifuged for 1min at 4000rpm, is sequentially centrifuged for 0.5min at 3500rpm, is centrifuged for 0.5min at 3000rpm and is centrifuged for 0.5min at 2500 rpm.
(3) Taking the centrifuged dairy product to be tested, setting the rotating speed to be 2000rpm by adopting a LUMiSizer X65 stability analyzer, setting the scanning time interval to be 8s, setting the total scanning times to be 220 times, setting the testing temperature to be 25 ℃, setting the light intensity factor to be 1.0, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 1.
Example 9 high viscosity samples
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the stirred yoghurt of the same batch in the example 7 as the dairy product to be detected.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and the pretreatment is carried out for a plurality of times by adopting a fast and slow centrifugation mode, and the dairy product is firstly centrifuged for 1min at 4000rpm and then centrifuged for 0.5min at 3500 rpm.
(3) Taking the centrifuged dairy product to be tested, setting the rotating speed to be 3000rpm, the scanning time interval to be 8s, the total scanning times to be 220 times, the testing temperature to be 25 ℃, the light intensity factor to be 1.0 by adopting a LUMiSizer X65 stability analyzer, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 1.
Example 10 highly viscous sample
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the stirred yoghurt of the same batch in the example 7 as the dairy product to be detected.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and is subjected to multiple times of pretreatment by adopting a fast and slow centrifugation mode, wherein the dairy product is firstly centrifuged for 1min at 4000rpm, is sequentially centrifuged for 0.5min at 3500rpm, is centrifuged for 0.5min at 3000rpm and is centrifuged for 0.5min at 2500 rpm.
(3) Taking the centrifuged dairy product to be tested, setting the rotating speed to be 2000rpm by adopting a LUMiSizer X65 stability analyzer, setting the scanning time interval to be 8s, setting the total scanning times to be 100 times, setting the testing temperature to be 25 ℃, setting the light intensity factor to be 1.0, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 2.
Example 11 high viscosity samples
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the stirred yoghurt of the same batch in the example 7 as the dairy product to be detected.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and is subjected to multiple times of pretreatment by adopting a fast and slow centrifugation mode, wherein the dairy product is firstly centrifuged for 1min at 4000rpm, is sequentially centrifuged for 0.5min at 3500rpm, is centrifuged for 0.5min at 3000rpm and is centrifuged for 0.5min at 2500 rpm.
(3) Taking the pretreated dairy product to be detected, adopting a LUMiSizer X65 stability analyzer, setting the rotating speed to be 2000rpm, the scanning time interval to be 8s, the total scanning times to be 300 times, the testing temperature to be 25 ℃, the light intensity factor to be 1.0, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 2.
Example 12 high viscosity samples
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the stirred yoghurt of the same batch in the example 7 as the dairy product to be detected.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and is subjected to multiple times of pretreatment by adopting a fast and slow centrifugation mode, wherein the dairy product is firstly centrifuged for 1min at 4000rpm, is sequentially centrifuged for 0.5min at 3500rpm, is centrifuged for 0.5min at 3000rpm and is centrifuged for 0.5min at 2500 rpm.
(3) Taking the centrifuged dairy product to be tested, setting the rotating speed to be 2000rpm by adopting a LUMiSizer X65 stability analyzer, setting the scanning time interval to be 8s, setting the total scanning times to be 220 times, setting the testing temperature to be 20 ℃, setting the light intensity factor to be 1.0, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 2.
Example 13 high viscosity sample
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) taking the stirred yoghurt of the same batch in the example 7 as the dairy product to be detected.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and is subjected to multiple times of pretreatment by adopting a fast and slow centrifugation mode, wherein the dairy product is firstly centrifuged for 1min at 4000rpm, is sequentially centrifuged for 0.5min at 3500rpm, is centrifuged for 0.5min at 3000rpm and is centrifuged for 0.5min at 2500 rpm.
(3) Taking the centrifuged dairy product to be tested, setting the rotating speed to be 2000rpm by adopting a LUMiSizer X65 stability analyzer, setting the scanning time interval to be 20s, setting the total scanning times to be 220 times, setting the testing temperature to be 30 ℃, setting the light intensity factor to be 1.0, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 2.
Example 14 highly viscous sample
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) and taking the commercially available stirred yogurt as the dairy product to be measured, repeatedly measuring for three times by using a viscometer and a rotor with a number T-C, and taking an average value to measure the viscosity of the stirred yogurt to be 14980 cp.
(2) A pretreatment step: 2.0g of the dairy product to be detected which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, and is subjected to multiple times of pretreatment by adopting a fast and slow centrifugation mode, wherein the dairy product is firstly centrifuged for 1min at 4000rpm, is sequentially centrifuged for 0.5min at 3500rpm, is centrifuged for 0.5min at 3000rpm and is centrifuged for 0.5min at 2500 rpm.
(3) Taking the pretreated dairy product to be detected, adopting a LUMiSizer X65 stability analyzer, setting the rotating speed to be 2000rpm, the scanning time interval to be 8s, the total scanning times to be 220 times, the testing temperature to be 25 ℃, the light intensity factor to be 1.0, repeatedly measuring each sample for three times, respectively reading the instability index of the product, and calculating the repeatability, the accuracy and the precision, wherein the result is shown in Table 2.
Example 15 Low viscosity sample
The embodiment provides a method for detecting the stability of a dairy product, which comprises the following steps:
(1) the measurement was repeated three times using a viscometer and an LV type rotor with a commercially available drinking type yogurt, and the average value was taken to obtain a milk product to be measured having a viscosity of 1950 cp.
(2) 2.0g of the dairy product to be tested which is uniformly mixed and has no bubbles is taken and loaded into a 2mm PC sample tube, a LUMiSizer X65 stability analyzer is adopted, the set rotating speed is 3500rpm, the scanning time interval is 15s, the total scanning frequency is 150 times, the testing temperature is 25 ℃, the light intensity factor is 1.0, each sample is repeatedly measured for three times, the instability index of the product is respectively read, and the repeatability, the accuracy and the precision are calculated, and the results are shown in Table 2.
Comparative example 1 centrifugal precipitation Rate
The comparative example provides a method for detecting the stability of a dairy product, which comprises the following steps:
accurately weighing mass M of blank centrifugal tube1Taking 30g of the same batch of milk as the milk product to be measured in the embodiment 1, adding the milk product to be measured into a centrifugal tube, and precisely weighing the mass M of the milk product to be measured and the mass M of the centrifugal tube2And carrying out centrifugal test for 37.5min under the test condition that the centrifugal rotating speed is 3500 rpm. After the measurement is finished, the supernatant is discarded, and the weight M of the sediment and the centrifugal tube is accurately weighed3The samples were tested in triplicate, the mean value was taken and the centrifugation and sedimentation rate was calculated according to the following formula. From the results of the repeated measurements, the reproducibility, accuracy and precision were calculated, and the results are shown in Table 1. (M) percent of centrifugal precipitation3-M1)/(M2-M1)×100％；M1The mass of the centrifuge tube; m2The total mass of the sample and the centrifuge tube; m3Is the total mass of the pellet and centrifuge tube.
Centrifugal water loss rate of viscosity sample in comparative example 2
The comparative example provides a method for detecting the stability of a dairy product, which comprises the following steps:
accurately weighing mass M of blank centrifugal tube1Taking 30g of the same batch of drinking yoghurt obtained in the embodiment 4 as the dairy product to be detected, adding the dairy product to be detected and the mass M of the centrifugal tube to be detected accurately2And carrying out centrifugal test for 30min under the test condition that the centrifugal rotating speed is 3000 rpm. After the measurement is finished, collecting the supernatant, and accurately weighing the weight M of the supernatant3The samples were tested in triplicate, the average value was taken and the centrifuge water loss rate was calculated according to the following formula. From the results of the repeated measurements, the reproducibility, accuracy and precision were calculated, and the results are shown in Table 1. Centrifugal water loss rate%3/(M2-M1)×100％；M1The mass of the centrifuge tube; m2The total mass of the sample and the centrifuge tube; m3Is the mass of the supernatant.
Comparative example 3 centrifugal Water loss Rate of high viscosity sample
The comparative example provides a method for detecting the stability of a dairy product, which comprises the following steps:
accurately weighing mass M of blank centrifugal tube1Taking 30g of the same batch of stirred yoghurt as in example 7 as the dairy product to be detected, adding the dairy product to be detected and the mass M of the centrifugal tube (the sample is not more than 35g) into the centrifugal tube, and accurately detecting the mass M of the dairy product to be detected and the mass M of the centrifugal tube2And carrying out centrifugal test for 30min under the test condition that the centrifugal rotating speed is 2000 rpm. After the measurement is finished, collecting the supernatant, and accurately weighing the weight M of the supernatant3The samples were tested in triplicate, averaged and the centrifuge water loss calculated. From the results of the repeated measurements, the reproducibility, accuracy and precision were calculated, and the results are shown in Table 1.
Comparative example 4
The comparative example provides a method for detecting the stability of a dairy product, which comprises the following steps:
taking the same batch of stirred yoghurt of example 7 as the dairy product to be measured, weighing 2.0g of the dairy product to be measured, loading the dairy product to be measured into a 2mm PC sample tube, measuring by adopting a LUMiZerX 65 stability analyzer under the conditions of set rotating speed of 2000rpm, scanning time interval of 8s, total scanning frequency of 220 times, test temperature of 25 ℃ and light intensity factor of 1.0, repeating the measurement for three times for each sample, respectively reading the instability index of the product, and calculating repeatability, accuracy and precision, wherein the result is shown in Table 2.
TABLE 1 test results of examples 1 to 9 and comparative examples 1 to 3
TABLE 2 test results of examples 10 to 15 and comparative examples 4 to 5
Combining the results of tables 1 and 2, it can be seen that the instability index of comparative example 4 without pretreatment has an RSD of 11.083%, which is significantly out of the error range of RSD, and the test results are unreliable. Compared with the comparative example 4, the embodiments 4 to 15 of the invention obviously improve the accuracy and precision of the testing method, expand the application range of the product, have simple and convenient operation, low cost and short testing time by pretreating the dairy product with higher viscosity.
As can be seen from the results in table 1 above and in fig. 1-9, the instability indexes measured by the methods of examples 1-3 of the present invention are close to their respective average values, which indicates that the methods of examples 1-3 are very reproducible, the SD of the instability indexes is 0.001% and is significantly less than 0.015% of the comparative example, which indicates that the accuracy of the examples is significantly improved, and the RSD of the instability indexes of examples 1 and 2 are 2.014% and 2.585% and are significantly less than 3.262% of the comparative example 1, which indicates that the precision of the examples 1 and 2 is significantly improved. Furthermore, the highest precision was achieved for example 2, which is consistent with the unstable profile showing that there was a slight fat float and minimal settling in the system, indicating that complete settling of the system had occurred and that the measured values were closer to the actual values. Therefore, compared with the traditional centrifugation method, the detection method provided by the invention has the advantages that the accuracy, precision and repeatability of the dairy product with lower viscosity are obviously improved.
As can be seen from the results in Table 1 above and from FIGS. 10-18, the instability indexes measured by the methods of examples 4-6 of the present invention are close to their respective average values, which indicates that the methods of examples 4-6 have good reproducibility, the SD of the instability indexes is 0.003-0.004%, which indicates that the accuracy of this example is significantly improved, and the RSD of the instability indexes of examples 4 and 5 is 0.740-1.788%, which is significantly lower than 3.062% of comparative example 2, which indicates that the precision of examples 4-6 is significantly improved, compared with comparative example 2. The precision of example 5 is highest, the phenomena of floating, elutriation and sinking of the particles of the product system can be clearly seen by a spectrum, and the spectrum represents that the product system is completely separated, which shows that the test condition is superior to other examples and comparative example 2 in the group. Therefore, compared with the traditional centrifugation method, the detection method provided by the invention has the advantages that the accuracy, precision and repeatability of the medium-viscosity dairy product are obviously improved.
As can be seen from the results in Table 1 above in conjunction with FIGS. 19-27, the instability indexes of examples 7-9 of the present invention are close to the average of the three tests compared to comparative example 3, indicating that the methods of examples 4-6 are very reproducible, the instability indexes of examples 8 and 9 both have an SD of 0.003%, indicating that the accuracy of examples 8 and 9 is significantly improved, and the instability indexes of examples 1 and 2 have an RSD of 0.898-2.291% which is significantly lower than 3.918% of comparative example 3, indicating that the precision of examples 7-9 is significantly improved. The precision of example 8 is highest, the phenomena of floating, elutriation and sinking of the particles of the product system can be clearly seen by a spectrum, and the spectrum represents that the product system is completely separated, which shows that the test condition is superior to other examples and comparative example 3 in the group. Therefore, compared with the traditional centrifugal method, the detection method provided by the invention has the advantages that the accuracy, precision and repeatability are obviously improved for the dairy product with higher viscosity.
As can be seen from the results of table 2 above in conjunction with the result graphs of examples 10 and 11, the instability index RSD of the screening results for the number of lines tested in examples 10 and 11 of the present invention is 1.038 to 1.243% compared to example 8 and comparative example 3, the accuracy is significantly lower than 3.918% of comparative example 3 and higher than 0.898% of the preferred embodiment, indicating that the results of examples 10 and 11 are significantly higher in accuracy than comparative example 3 but lower than example 8.
As can be seen from the results of table 2 above in conjunction with the result graphs of examples 12 and 13, the instability index RSD of the screening results for the test temperature in examples 12 and 13 of the present invention is 1.006 to 1.038% compared to example 8 and comparative example 3, the accuracy is significantly lower than 3.918% of comparative example 3 and higher than 0.898% of example 8, indicating that the results of examples 12 and 13 are more accurate than comparative example 3 but lower than example 8. Analysis results show that the link time of temperature balance in actual operation is considered comprehensively, the operation is more convenient under the room temperature (25 ℃) condition, and the consumed time is shorter.
As can be seen from the results of example 14 of table 2 above, the results show that the instability index of example 14 has an RSD of 1.189% and a precision of 3.918% higher than that of comparative example 3 and slightly lower than 0.898% of preferred embodiment 3, compared to example 8 and comparative example 3 for the highly viscous sample, indicating that the test method of example 14 has higher accuracy and precision for the highly viscous sample.
As can be seen from the results of example 15 of table 2 above, the results show that the RSD of the instability index of example 15 is 1.613% significantly lower than the instability indexes of 2.014% to 3.262% for example 1 and comparative 1, compared to example 1 and comparative 1, which are low viscosity samples. The test method of example 15 is demonstrated to have high accuracy and precision for low viscosity samples.
And (3) an observation method: taking the milk, the drinking yoghurt and the stirring yoghurt of each embodiment, respectively placing for 6 months at normal temperature, observing that no serious phenomena of water separation, fat floating, flocculation or precipitation occur, and showing that the milk products are stable dairy products, wherein the detection method of the embodiments 1-15 accords with the observation result, and the method of the embodiments is accurate and reliable.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for detecting the stability of dairy products comprises the following steps,
(1) determining the viscosity eta of the dairy product to be detected;
(2) a pretreatment step: when eta is more than 2000 and less than 10000cp, centrifuging the dairy product to be detected for 0.5-3min at 4000rpm of 2500-; when eta is more than or equal to 10000 and less than 15000cp, centrifuging the dairy product to be detected for 0.5-3min at 3500-;
(3) instability index determination step: and (3) measuring the light transmittance change of the dairy product to be measured with eta less than or equal to 2000cp, the dairy product to be measured with eta less than or equal to 2000cp after the pretreatment in the step (2) or the dairy product to be measured with eta less than or equal to 10000cp after the pretreatment in the step (2) at the rotation speed of 1000-4000rpm by adopting a stability analyzer through infrared scanning to obtain the instability index.
2. The method for detecting the stability of the dairy product according to claim 1, wherein in the step (2), the pretreatment step for the dairy product to be detected with the eta <15000cp of 10000 ≤ is to centrifuge at 4000rpm for 0.5-2min, then sequentially centrifuge at 3500rpm for 0.5-1min, 3000rpm for 0.5-1min, and 2500rpm for 0.5-1 min.
3. The method for detecting the stability of the dairy product according to claim 1, wherein in the step (2), the pretreatment step for the dairy product to be detected with 2000< η <10000cp is to centrifuge at 4000rpm for 0.5-2min and then at 3500rpm for 0.5-1 min.
4. The method for detecting the stability of a dairy product as claimed in any one of claims 1-3, wherein in step (3), the testing temperature is 20-35 ℃, and the scanning is performed every 5-20s for 100 times and 300 times.
5. The method for detecting the stability of a dairy product as claimed in any one of claims 1 to 4, wherein in the step (3), the testing rotation speed for the dairy product to be detected with η ≦ 2000cp is 3000-4000 rpm; for the dairy product to be tested with eta <10000cp of 2000, the testing rotating speed is 2000-4000 rpm; for the dairy product to be tested with the eta of more than or equal to 10000 and less than 15000cp, the test rotating speed is 1000-3000 rpm.
6. The method for detecting the stability of the dairy product according to any one of claims 1 to 5, wherein for the dairy product to be detected with eta ≦ 2000cp, the test conditions in the step (3) are: the rotating speed is 3500rpm, the testing temperature is 25 ℃, the scanning is carried out once every 15s for 150 times, and the light intensity factor is 1.0.
7. The method for detecting the stability of the dairy product according to any one of claims 1 to 6, wherein for the dairy product to be detected with 2000< η <10000cp, the test conditions in the step (3) are as follows: the rotating speed is 3000rpm, the testing temperature is 25 ℃, the scanning is carried out once every 10s for 180 times, and the light intensity factor is 1.0.
8. The method for detecting the stability of the dairy product according to any one of claims 1 to 7, wherein the test conditions in the step (3) for the dairy product to be detected with 10000 ≤ η <15000cp are as follows: the rotating speed is 2000rpm, the testing temperature is 25 ℃, the scanning is carried out once every 8s, the total scanning is 220 times, and the light intensity factor is 1.0.
9. Method for testing the stability of a dairy product according to any one of claims 1 to 8, wherein the stability analyzer is a LUMi-Sizer stability analyzer and/or a LUMiFuge stability analyzer.
10. The method for detecting the stability of the dairy product according to any one of claims 1 to 9, wherein the dairy product is at least one of milk, recombined milk, milk beverage and fermented milk.
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