CN116482284A - Human milk characteristic fatty acid fingerprint and application thereof in authenticity identification - Google Patents
Human milk characteristic fatty acid fingerprint and application thereof in authenticity identification Download PDFInfo
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- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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Abstract
The invention discloses a human milk characteristic fatty acid fingerprint and application thereof in authenticity identification, and belongs to the technical field of food analysis. The characteristic fatty acid finger print of the milk of the invention adopts C8:0 and C14:1 in human milkcis‑9、C15:0、C15:0 anteiso、C18:2 c9t11(CLA n7)、C18:2 c9c12(LA)、C20:1 cis‑11Based on eight characteristic fatty acids of C22:6c4c7c10c13c16c19 (DHA), standard human milk fingerprint patterns based on the ratios of C8:0/LA, C8:0/DHA, C14:1cis-9/C20:1cis-11, C15:0/DHA and C15:0 antais/C20:1 cis-11 and CLA/LA are constructed. And (3) measuring the content of characteristic fatty acid in the sample to be measured, calculating a corresponding ratio, comparing with a standard human milk fingerprint, and judging that the sample is not completely human milk when any ratio exceeds a characteristic range. The human milk characteristic fatty acid fingerprint can be judged in a multi-dimensional manner by using 6 standard indexes, so that the authenticity of the human milk can be rapidly and accurately identified. Only the fatty acid content needs to be measured, and the method is simple, convenient and quick. The fingerprint spectrum is used for identifying the authenticity with strong applicability toThe historical data, the literature data and the like can be used for judging whether the sample is absent, and the traceability is strong.
Description
Technical Field
The invention belongs to the technical field of food analysis, and particularly relates to a human milk characteristic fatty acid fingerprint and application thereof in authenticity identification.
Background
Milk is a basic dietary source for mammalian pups and can provide a range of nutrients beneficial to human health including lipids, proteins, bioactive peptides, minerals, vitamins, etc. (Liu et al, 2018). The dairy products in China are rich in variety, and besides common cow milk (Holstein cow milk and silk cow milk) in the market, the dairy products also have characteristic milk such as goat milk, buffalo milk, yak milk and the like. Human milk is always considered to be the most favorable food for the growth and development of human infants compared to animal milk. Therefore, the research on the nutrition value of the human milk becomes an important marker post for evaluating the nutrition quality of the dairy products, and is also a reference basis for the formula of the infant milk powder. However, human milk samples are extremely difficult to obtain for current ethical reasons, which to some extent restricts studies related to human milk, such as medicine, physiology, food science, forensics, etc. In this case, it is particularly important to ensure the authenticity of the human milk sample. The counterfeiting or doping of animal milk into human milk will bring about a deviation in direction for related scientific research and investigation evidence.
Currently, milk authenticity identification can be achieved by detecting proteins or genes in milk. Shalma et al (2021) used non-immunoglobulin antigens in milk as an indicator and could identify milk adulteration as low as 5% in buffalo milk by immunization methods. Malo et al (2018) used immunoglobulins in milk as an indicator and identified milk adulteration as low as 1% in goat milk, sheep milk, buffalo milk by immunization methods. Liu et al (2019) used casein in milk as an indicator, and could adulterate as low as 0.07% of milk in identified goat milk by immunization, while Ren et al (2014) also identified as low as 1% of milk in yak milk using casein in milk. Trimboli et al (2019) detected the alpha-lactalbumin content in milk by capillary electrophoresis, and used alpha-lactalbumin as an indicator to identify milk adulteration as low as 1% in buffalo milk and to quantify the adulteration level of 3.1% or more in buffalo milk. Chen et al (2016) use a proteomic method to qualitatively and quantitatively analyze cow milk doped in goat milk or sheep milk using beta-lactoglobulin as an indicator. De et al (2011) uses mitochondrial DNA circular fragments as target sequences, utilizes PCR technology to amplify 126bp and 226bp specific PCR products of cow milk and buffalo milk respectively, and utilizes species specific DNA sequences to identify milk adulteration as low as 0.01% in buffalo milk. However, the processes such as homogenization and heat treatment of dairy products have great damage to proteins and genes, and the milk has a wide range of protein content and a large number of interference factors. Therefore, the identification method based on the protein characteristics has low sensitivity to the species difference, and is easy to generate false positive results, while the identification method based on the species gene difference has high sensitivity, but is time-consuming and expensive, has high application threshold and is difficult to popularize.
In addition, milk authenticity identification can also be achieved by cluster analysis of specific nutritional components in milk. Pereira et al (2020) determined the total content of fat and protein in milk and goat milk based on near infrared spectroscopy and established a PLS-DA model to identify milk added to goat milk at levels as low as 1.0154g/100 g. Sen et al (2021) based on fourier transform infrared spectroscopy to determine total fat, protein, lactose and non-fat solids content of cow milk, buffalo milk and goat milk, established an OPLS-DA model to identify two milk mixtures of cow milk-goat milk and cow milk at a mixing level higher than 5% with discriminant analysis at 93% and 91% accuracy, respectively. Zhang Xin et al (2018) determine fatty acid content of cow milk and mare milk based on gas chromatography, analyze mixed samples of cow milk and mare milk by adopting PCA, SIMCA and PLS models, clarify feasibility of fatty acid fingerprint to identify authenticity of characteristic milk, and can identify adulteration of cow milk as low as 10% in mare milk.
The raw milk has rich fatty acid species, and the composition and content of the fatty acid in the raw milk of different species are greatly different. The fatty acid fingerprint spectrum refers to the composition profile and content characteristics of all fatty acids in milk, and is used as a species difference or specificity recognition technology, so that the identification of the authenticity of the dairy products is more accurate and reliable. However, the results of fatty acid measurement are currently presented in terms of relative content, which requires an area normalized quantification of all fatty acids in milk (Liu et al, 2018), which greatly increases the analysis time. The characteristic fatty acid ratio is selected, so that the analysis process can be simplified, the efficiency of the authenticity identification is improved, the difference is maximized, and the accuracy of the authenticity identification is improved. It was found that the ratios of C10:0/C8:0, C12:0/C10:0, C14:0/C12:0 and C14:0/C18:1 fatty acids can discriminate the incorporation of tallow and lard into milk fat (Anmat, 2011), but that the method of Rebechi et al (2016) can only identify tallow or lard with a milk fat incorporation of more than 15% and has insufficient detection sensitivity.
The method can realize the identification of dairy adulteration to a certain extent, but has certain limitation in applying the method to the identification of human milk authenticity, such as complex operation, long operation time, high analysis cost, low sensitivity, poor applicability and the like because pretreatment such as separation, extraction and the like is needed before the measurement. The human milk authenticity identification method in the prior art has less research, and has no authenticity identification method with strong applicability and traceability for human milk authenticity. Therefore, a human milk authenticity identification method capable of accurately identifying the authenticity, simplicity and convenience in operation and strong applicability and traceability of human milk and products thereof needs to be developed.
Disclosure of Invention
In order to overcome the problems of hysteresis of the dairy product authenticity identification method in the prior art and no identification method with strong applicability and traceability for human milk authenticity identification. The invention aims to provide a set of characteristic ranges of characteristic fatty acid ratios in human milk, and a fingerprint of the human milk is constructed according to the characteristic ranges of the characteristic fatty acid ratios and is applied to the authenticity identification of the human milk and related products.
The invention has the following ideas: compared with animal milk such as cow milk, buffalo milk, yak milk, sheep milk, donkey milk, camel milk, etc., the human milk has higher contents of fatty acids such as LA, DHA, C20:1c11, etc., while the human milk has lower contents of fatty acids such as C8:0, C15:0 antais, C14:1c9, CLA, etc. The invention utilizes a large amount of experimental accumulation and back regulation data of earlier-stage research to count and screen various fatty acid ratios, and screens out several characteristic fatty acid ratios which have extremely small values in human milk and large differences with other animal milks. For each characteristic fatty acid ratio, calculating a characteristic range in human milk by adopting an AVG (average value) +/-3 XSD (standard deviation) mode, wherein the confidence coefficient reaches 99%, and manufacturing a radar graph to form a fingerprint. And (3) measuring and calculating the characteristic fatty acid ratio value of the milk sample to be measured, and then comparing the characteristic fatty acid ratio value with the fingerprint spectrum to identify the authenticity.
The specific technical scheme of the invention is as follows:
a human milk characteristic fatty acid fingerprint, wherein the human milk characteristic fatty acid is: c8:0, C14:1cis-9, C15:0 antais, C18:2c9t11 (CLA), C18:2c9c12 (LA), C20:1cis-11, C22:6c4c7c10c16c19 (DHA).
A human milk characteristic fatty acid fingerprint is constructed based on the ratio values of C8:0/LA, C8:0/DHA, C14:1cis-9/C20:1cis-11, C15:0/DHA and C15:0 antais/C20:1 cis-11 and CLA/LA 6 fatty acids in human milk, and the characteristic fatty acid ratio ranges are as follows:
the human milk authenticity identification method applying the human milk characteristic fatty acid fingerprint comprises the following steps:
s1, measuring the content of characteristic fatty acid in a sample to be measured, and calculating the corresponding characteristic fatty acid ratio of human milk;
s2, comparing the corresponding fatty acid ratio calculated in the step S1 with a characteristic fatty acid fingerprint of human milk, and judging that the sample is not completely human milk and is counterfeit or adulterated when any characteristic fatty acid ratio exceeds a characteristic range, namely is out of a radar chart confidence range.
Preferably, the characteristic fatty acid content in the human milk sample to be measured in the step S1 is measured by gas chromatography or gas chromatography-mass spectrometry.
Preferably, the results of calculating the corresponding fatty acid ratio as described in step S1 are in terms of relative values (% total fatty acids).
Preferably, the results of calculating the corresponding fatty acid ratio as described in step S1 are in absolute values (mg/L milk).
Compared with the prior art, the invention has the beneficial effects that:
(1) Fingerprint characteristics (exclusivity): the characteristic fatty acid ratio value selected in the invention has obvious fingerprint characteristics. The above ratios are all minimum values compared to other animal milks. The 6 indexes are judged from multiple dimensions, so that other animal milks can be rapidly and accurately distinguished.
(2) The method is simple and quick: compared with the immune method for measuring protein or nucleic acid, the method has the advantages that the measurement of fatty acid content is simpler, and the measurement can be completed within 4-6 hours. More importantly, the fatty acid is used as a basic nutrition index, belongs to a normal measurement index of a milk sample, and therefore, the conclusion of the identification of the human milk authenticity can be obtained only by analyzing the existing detection result by using the method.
(3) The applicability is strong: compared with the immune method for measuring protein or nucleic acid, the method has the advantages of low technical threshold for measuring fatty acid content and low cost. The results may be measured by gas chromatography or gas chromatography-mass spectrometry, or may be obtained by an infrared rapid measurement device.
(4) The traceability is strong: the human milk authenticity identification method based on the characteristic fatty acid fingerprint can be used for judging through data, and can be used for judging whether historical data, literature data and the like are sample-free.
Drawings
Fig. 1 is a radar chart of a characteristic fatty acid ratio range of a characteristic fatty acid fingerprint of human milk of the present invention.
Detailed Description
The present invention will now be further described in connection with specific embodiments in order to enable those skilled in the art to better understand the invention. The following examples are only illustrative of the present invention and are not intended to limit the scope of the invention.
Example 1
Based on eight characteristic fatty acids of C8:0, C14:1cis-9, C15:0 antais, C18:2c9t11 (CLA), C18:2c9c12 (LA), C20:1cis-11, C22:6c4c7c10c16c16c19 (DHA) in human milk, standard human milk characteristic fatty acid finger print based on six ratios of C8:0/LA, C8:0/DHA, C14:1cis-9/C20:1cis-11, C15:0/DHA, C15:0 antais/C20:1 cis-11, CLA/LA were constructed, the human milk characteristic fatty acid ratio ranges are shown in Table 1:
table 1: characteristic range of characteristic fatty acid ratio in human milk
And drawing a radar chart of the characteristic fatty acid ratio range of the human milk according to the characteristic fatty acid ratio range, wherein the radar chart is shown in figure 1.
Example 2
Taking 59 Holstein cow milk for verification analysis, measuring the content of characteristic fatty acid in a sample, calculating the corresponding fatty acid ratio, comparing with the standard human milk fingerprint constructed in the embodiment 1, and judging that the sample is not completely human milk and is fake or adulterated when any characteristic fatty acid ratio exceeds a characteristic range, namely is out of a radar chart confidence range, wherein the results are shown in tables 2-1 and 2-2.
Table 2-1 characteristic fatty acid content of milk counterfeits or adulterants into human milk (% total fatty acids, n=59)
Note that: the DHA content in animal milk is extremely low, and when the content is lower than the detection limit, the values of C8:0/DHA and C15:0/DHA are extremely large, and the minimum value and the identifiable adulteration ratio are calculated by using the quantitative limit of DHA as 0.01 percent FA.
Table 2-2 authenticity verification of milk counterfeits or dopings of Holstein cows' milk (n=59)
The test results show that all milk samples can be judged to be not in accordance with the characteristics of human milk, and the milk of Holstein cow doped with 1.1% in human milk can be identified.
Example 3
Taking 32 parts of Dairy cow milk from Juan san, performing verification analysis, measuring the content of characteristic fatty acid in a sample, calculating the corresponding fatty acid ratio, comparing with the standard human milk fingerprint constructed in the embodiment 1, and judging that the sample is not completely human milk and is counterfeit or adulterated when any characteristic fatty acid ratio exceeds a characteristic range, namely is out of a radar chart confidence range, wherein the results are shown in tables 3-1 and 3-2.
Table 3-1 juan san dairy cow milk counterfeits or is doped with characteristic fatty acid content of human milk (% total fatty acids, n=32)
Note that: the DHA content in animal milk is extremely low, and when the content is lower than the detection limit, the values of C8:0/DHA and C15:0/DHA are extremely large, and the doping proportion can be identified by calculating the quantitative limit of DHA as 0.01 percent FA.
Table 3-2 authentication of the authenticity of Dairy cow milk counterfeiting or doping into human milk (n=32)
The test results show that all milk samples can be judged to be not in accordance with the characteristics of human milk, and the 1.2% silk cow milk doped in the human milk can be identified.
Example 4
11 parts of buffalo milk is taken for verification analysis, the content of characteristic fatty acid in a sample is measured, the corresponding fatty acid ratio is calculated, the fatty acid ratio is compared with the standard human milk fingerprint constructed in the embodiment 1, when any characteristic fatty acid ratio value exceeds a characteristic range, namely is out of a confidence range of a radar chart, the sample is judged to be not completely human milk, and the result is shown in tables 4-1 and 4-2.
Table 4-1 buffalo milk counterfeiting or doping into human milk characteristic fatty acid content (% total fatty acids, n=11)
Note that: the DHA content in animal milk is extremely low, and when the content is lower than the detection limit, the values of C8:0/DHA and C15:0/DHA are extremely large, and the doping proportion can be identified by calculating the quantitative limit of DHA as 0.01 percent FA.
Table 4-2 authenticity verification of buffalo milk counterfeit or doped into human milk (n=11)
The test results show that all milk samples can be judged to be not in accordance with the characteristics of human milk, and the buffalo milk doped with 1.5% in the human milk can be identified.
Example 5
And (3) taking 25 parts of yak milk for verification analysis, measuring the content of characteristic fatty acid in a sample, calculating the corresponding fatty acid ratio, comparing with the standard human milk fingerprint constructed in the embodiment 1, and judging that the sample is not completely human milk when any characteristic fatty acid ratio exceeds a characteristic range, namely is out of a confidence range of a radar chart, wherein the result is shown in tables 5-1 and 5-2.
Table 5-1 characteristic fatty acid content of milk counterfeited or spiked into human milk (% total fatty acids, n=25)
Note that: the DHA content in animal milk is extremely low, and when the content is lower than the detection limit, the values of C8:0/DHA and C15:0/DHA are extremely large, and the doping proportion can be identified by calculating the quantitative limit of DHA as 0.01 percent FA.
Table 5-2 authenticity verification of yak milk counterfeit or doped into human milk (n=25)
The test results show that all milk samples can be judged to be not in accordance with the characteristics of the human milk, and the yak milk doped with 2.2% in the human milk can be identified.
Example 6
38 parts of goat milk are taken for verification analysis, the content of characteristic fatty acid in a sample is measured, the corresponding fatty acid ratio is calculated, the characteristic fatty acid ratio is compared with the standard human milk fingerprint constructed in the embodiment 1, when any characteristic fatty acid ratio value exceeds a characteristic range, namely is out of a confidence range of a radar chart, the sample is judged to be not completely human milk, and the result is shown in tables 6-1 and 6-2.
Table 6-1 characteristic fatty acid content of goat milk counterfeited or spiked into human milk (% total fatty acids, n=38)
Note that: the DHA content in animal milk is extremely low, and when the content is lower than the detection limit, the values of C8:0/DHA and C15:0/DHA are extremely large, and the doping proportion can be identified by calculating the quantitative limit of DHA as 0.01 percent FA.
Table 6-2 authenticity verification of goat milk counterfeit or adulterated into human milk (n=38)
The test results show that all milk samples can be judged to be not in accordance with the characteristics of human milk, and the goat milk doped with 2.5% in the human milk can be identified.
Example 7
And (3) taking 27 parts of camel milk for verification analysis, measuring the content of characteristic fatty acid in a sample, calculating the corresponding fatty acid ratio, comparing with the standard human milk fingerprint constructed in the example 1, and judging that the sample is not completely human milk when any characteristic fatty acid ratio exceeds a characteristic range, namely is out of a confidence range of a radar chart, wherein the result is shown in tables 7-1 and 7-2.
Table 7-1 camel milk counterfeits or is doped with characteristic fatty acid content of human milk (% total fatty acids, n=27)
Note that: the DHA content in animal milk is extremely low, and when the content is lower than the detection limit, the values of C8:0/DHA and C15:0/DHA are extremely large, and the doping proportion can be identified by calculating the quantitative limit of DHA as 0.01 percent FA.
Table 7-2 authenticity verification of camel milk counterfeit or doped into human milk (n=27)
The test results show that all milk samples can be judged to be not in accordance with the characteristics of human milk, and 4.5% of camel milk doped in human milk can be identified.
Example 8
And (3) taking 15 parts of donkey milk for verification analysis, measuring the content of characteristic fatty acid in a sample, calculating the corresponding fatty acid ratio, comparing with the standard human milk fingerprint constructed in the embodiment 1, and judging that the sample is not completely human milk when any characteristic fatty acid ratio exceeds a characteristic range, namely is out of a confidence range of a radar chart, wherein the result is shown in tables 8-1 and 8-2.
Table 8-1 donkey milk counterfeiting or doping into human milk characteristic fatty acid content (% total fatty acids, n=15)
Note that: the DHA content in animal milk is extremely low, and when the content is lower than the detection limit, the values of C8:0/DHA and C15:0/DHA are extremely large, and the doping proportion can be identified by calculating the quantitative limit of DHA as 0.01 percent FA.
Table 8-2 identification of authenticity of donkey milk counterfeit or doped into human milk (n=15)
The test results show that all milk samples can be judged to be not in accordance with the characteristics of human milk, and the human milk doped with 0.3% of human milk can be identified.
In summary, the human milk authenticity identification method based on the characteristic fatty acid fingerprint spectrum of the method is utilized to verify 59 parts of Holstein cow milk, 32 parts of Shanzan cow milk, 11 parts of buffalo milk, 25 parts of yak milk, 38 parts of goat milk, 27 parts of camel milk and 15 parts of human milk samples, and 207 other animal milk samples have characteristic fatty acid ratio values exceeding the characteristic range of human milk, and the difference identification rate is 100%; the human milk can be effectively identified by doping more than 0.3 to 4.5 percent of other animal milk.
Claims (6)
1. The characteristic fatty acid finger print of the human milk is characterized in that the characteristic fatty acid of the human milk is as follows: c8:0, C14:1cis-9、C15:0、C15:0 anteiso、C18:2 c9t11、C18:2 c9c12、C20:1 cis-11、C22:6 c4c7c10c13c16c19。
2. The human milk characteristic fatty acid fingerprint according to claim 1, wherein the characteristic fatty acid ratio ranges from:
C8:0/ C18:2 c9c12 0～0.010；
C8:0/ C22:6 c4c7c10c13c16c19 0～1.071；
C14:1 cis-9/C20:1 cis-11 0～0.537；
C15:0/ C22:6 c4c7c10c13c16c19 0～1.236；
C15:0 anteiso/C20:1 cis-11 0～0.333；
C18:2 c9t11/ C18:2 c9c12 0～0.022。
3. a human milk authenticity identification method using the human milk characteristic fatty acid fingerprint according to any one of claims 1 to 2, characterized by comprising the steps of:
s1, measuring the content of characteristic fatty acid in a sample to be measured, and calculating the corresponding characteristic fatty acid ratio of human milk;
s2, comparing the corresponding fatty acid ratio calculated in the step S1 with a characteristic fatty acid fingerprint of human milk, and judging that the sample is not completely human milk and is counterfeit or adulterated when any characteristic fatty acid ratio exceeds a characteristic range, namely is out of a radar chart confidence range.
4. A method for verifying the authenticity of human milk according to claim 3, wherein: and (3) determining the characteristic fatty acid content in the human milk sample to be tested in the step (S1) by using a gas chromatography method or a gas chromatography-mass spectrometry method.
5. A method for verifying the authenticity of human milk according to claim 3, wherein: the results of calculating the corresponding fatty acid ratio as described in step S1 are in terms of relative values.
6. A method for verifying the authenticity of human milk according to claim 3, wherein: the result of calculating the corresponding fatty acid ratio in step S1 is in absolute value.
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| CN116660442A (en) * | 2023-08-01 | 2023-08-29 | 中国农业科学院北京畜牧兽医研究所 | Identification method for counterfeit yak milk or other animal milk doped in yak milk |
| CN116660443A (en) * | 2023-08-01 | 2023-08-29 | 中国农业科学院北京畜牧兽医研究所 | Identification method for counterfeit camel milk or whether other animal milk is doped in camel milk |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116660442A (en) * | 2023-08-01 | 2023-08-29 | 中国农业科学院北京畜牧兽医研究所 | Identification method for counterfeit yak milk or other animal milk doped in yak milk |
| CN116660443A (en) * | 2023-08-01 | 2023-08-29 | 中国农业科学院北京畜牧兽医研究所 | Identification method for counterfeit camel milk or whether other animal milk is doped in camel milk |
| CN116660443B (en) * | 2023-08-01 | 2023-10-13 | 中国农业科学院北京畜牧兽医研究所 | Identification method for counterfeit camel milk or whether other animal milk is doped in camel milk |
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