CN112578053A - Method for judging adulteration of goat milk formula milk powder - Google Patents
Method for judging adulteration of goat milk formula milk powder Download PDFInfo
- Publication number
- CN112578053A CN112578053A CN202011573090.5A CN202011573090A CN112578053A CN 112578053 A CN112578053 A CN 112578053A CN 202011573090 A CN202011573090 A CN 202011573090A CN 112578053 A CN112578053 A CN 112578053A
- Authority
- CN
- China
- Prior art keywords
- milk
- milk powder
- adulterated
- aroma compounds
- goat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 225
- 239000008267 milk Substances 0.000 title claims abstract description 202
- 210000004080 milk Anatomy 0.000 title claims abstract description 202
- 235000013336 milk Nutrition 0.000 title claims abstract description 200
- 235000020210 goat's milk formula Nutrition 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 47
- 150000001875 compounds Chemical class 0.000 claims abstract description 147
- 235000020205 cow's milk formula Nutrition 0.000 claims abstract description 55
- 235000020251 goat milk Nutrition 0.000 claims abstract description 35
- 238000001228 spectrum Methods 0.000 claims abstract description 14
- 238000004817 gas chromatography Methods 0.000 claims abstract description 12
- 239000000796 flavoring agent Substances 0.000 claims abstract description 10
- 238000012216 screening Methods 0.000 claims abstract description 6
- 235000020610 powder formula Nutrition 0.000 claims abstract description 3
- 235000013350 formula milk Nutrition 0.000 claims description 59
- 239000000203 mixture Substances 0.000 claims description 33
- 238000000513 principal component analysis Methods 0.000 claims description 26
- 238000001514 detection method Methods 0.000 claims description 23
- 238000010586 diagram Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 13
- 235000020244 animal milk Nutrition 0.000 claims description 10
- 238000002470 solid-phase micro-extraction Methods 0.000 claims description 9
- BYGQBDHUGHBGMD-UHFFFAOYSA-N 2-methylbutanal Chemical compound CCC(C)C=O BYGQBDHUGHBGMD-UHFFFAOYSA-N 0.000 claims description 8
- 238000001819 mass spectrum Methods 0.000 claims description 8
- VSMOENVRRABVKN-UHFFFAOYSA-N oct-1-en-3-ol Chemical compound CCCCCC(O)C=C VSMOENVRRABVKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000001893 (2R)-2-methylbutanal Substances 0.000 claims description 4
- LVBXEMGDVWVTGY-VOTSOKGWSA-N (E)-oct-2-enal Chemical compound CCCCC\C=C\C=O LVBXEMGDVWVTGY-VOTSOKGWSA-N 0.000 claims description 4
- VSMOENVRRABVKN-MRVPVSSYSA-N 1-Octen-3-ol Natural products CCCCC[C@H](O)C=C VSMOENVRRABVKN-MRVPVSSYSA-N 0.000 claims description 4
- YDXQPTHHAPCTPP-UHFFFAOYSA-N 3-Octen-1-ol Natural products CCCCC=CCCO YDXQPTHHAPCTPP-UHFFFAOYSA-N 0.000 claims description 4
- XEAMDSXSXYAICO-UHFFFAOYSA-N Heptyl formate Chemical compound CCCCCCCOC=O XEAMDSXSXYAICO-UHFFFAOYSA-N 0.000 claims description 4
- 238000010239 partial least squares discriminant analysis Methods 0.000 claims description 4
- LVBXEMGDVWVTGY-UHFFFAOYSA-N trans-2-octenal Natural products CCCCCC=CC=O LVBXEMGDVWVTGY-UHFFFAOYSA-N 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- JZQKTMZYLHNFPL-ANYPYVPJSA-N (2e)-deca-2,4-dienal Chemical compound CCCCCC=C\C=C\C=O JZQKTMZYLHNFPL-ANYPYVPJSA-N 0.000 claims 1
- 235000020247 cow milk Nutrition 0.000 abstract description 23
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000012847 principal component analysis method Methods 0.000 abstract description 2
- 235000020256 human milk Nutrition 0.000 description 9
- 210000004251 human milk Anatomy 0.000 description 9
- 235000013305 food Nutrition 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 235000013365 dairy product Nutrition 0.000 description 4
- 238000007405 data analysis Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 235000015097 nutrients Nutrition 0.000 description 4
- 235000016709 nutrition Nutrition 0.000 description 4
- 238000004445 quantitative analysis Methods 0.000 description 4
- 235000020254 sheep milk Nutrition 0.000 description 4
- NUBWFSDCZULDCI-ANYPYVPJSA-N (2e)-deca-2,4-dien-1-ol Chemical compound CCCCCC=C\C=C\CO NUBWFSDCZULDCI-ANYPYVPJSA-N 0.000 description 3
- 206010020751 Hypersensitivity Diseases 0.000 description 3
- 208000026935 allergic disease Diseases 0.000 description 3
- 230000007815 allergy Effects 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 235000018102 proteins Nutrition 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XYYMFUCZDNNGFS-UHFFFAOYSA-N 2-methylheptan-3-one Chemical compound CCCCC(=O)C(C)C XYYMFUCZDNNGFS-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000000413 hydrolysate Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000035764 nutrition Effects 0.000 description 2
- TZMFJUDUGYTVRY-UHFFFAOYSA-N pentane-2,3-dione Chemical compound CCC(=O)C(C)=O TZMFJUDUGYTVRY-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 235000020613 types of formula milk Nutrition 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 102000009366 Alpha-s1 casein Human genes 0.000 description 1
- 108050000244 Alpha-s1 casein Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 108060003951 Immunoglobulin Proteins 0.000 description 1
- 208000009793 Milk Hypersensitivity Diseases 0.000 description 1
- 201000010859 Milk allergy Diseases 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 108010046377 Whey Proteins Proteins 0.000 description 1
- 102000007544 Whey Proteins Human genes 0.000 description 1
- 206010000059 abdominal discomfort Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000013566 allergen Substances 0.000 description 1
- 230000000172 allergic effect Effects 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 201000005356 cow milk allergy Diseases 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000020774 essential nutrients Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000001785 headspace extraction Methods 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 102000018358 immunoglobulin Human genes 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000002331 protein detection Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 235000021119 whey protein Nutrition 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7206—Mass spectrometers interfaced to gas chromatograph
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Library & Information Science (AREA)
- Engineering & Computer Science (AREA)
- Dairy Products (AREA)
Abstract
The invention aims to provide a convenient method for detecting adulteration of goat milk formula milk powder, which can accurately judge whether adulteration milk powder of cow milk powder is added in the goat milk formula milk powder or goat milk formula milk powder is faked without goat milk, and comprises the following steps: establishing a fingerprint spectrum library of aroma compounds in the non-adulterated goat milk formula milk powder and a fingerprint spectrum library of aroma compounds in the non-adulterated cow milk formula milk powder by gas chromatography, and screening out characteristic aroma compounds in the non-adulterated goat milk and cow milk formula milk powder. And determining an index aroma compound for identifying the goat milk formula milk powder by using least square discriminant analysis. And comparing the measured aroma compounds in the sample to be detected with the index aroma compounds in the non-adulterated goat milk and cow milk formula milk powder, determining whether the sample to be detected contains goat milk or not, determining whether the sample to be detected is adulterated or not, and judging more intuitively and quickly by combining a principal component analysis method.
Description
Technical Field
The invention belongs to the field of food science and technology, and particularly relates to a method for identifying whether goat milk formula milk powder is adulterated.
Background
The infant is a special group, while the breast milk is the most ideal food for the infant, and not only can the breast milk provide a nutrient source, but also contains biological components for promoting the normal growth and development of the infant. However, for various reasons, the rate of breast feeding for infants tends to decrease year by year, and under the condition of no breast milk or insufficient breast milk, the infant formula milk powder is the most important daily food source for infants as a breast milk substitute.
The research and production of infant formula milk powder in China are late, and the infant formula milk powder mainly based on cow milk is used at present. Cow milk is rich in nutrition and wide in source, and is always considered to be a good choice for infant formula milk powder base materials. However, in recent years, as the number of allergy cases caused by cow milk infant formula milk powder is increasing, people pay more and more attention to concepts such as nutrition and health. Therefore, the goat milk with rich nutritive value and low sensitization rate and the formula milk powder taking the goat milk as the main raw material are widely concerned by people.
The goat milk is a complete nutritional food, and is rich in essential nutrients such as protein, fat, minerals, vitamins, etc., which can promote human growth and development and maintain health. The goat milk contains more than 200 nutrient substances and bioactive factors, the protein and fat structures of the goat milk are very similar to those of the breast milk, the proportion of each nutrient is similar to that of the breast milk, and the goat milk is a milk product which is discovered at present and has the nutrient components closest to the breast milk. In addition, the protein composition in the goat milk is obviously different from that in the cow milk, the goat milk contains a large amount of whey protein and immunoglobulin, and the content of alpha-S1 casein which is easy to cause allergy is far lower than that of cow milk, so that the goat milk is not easy to cause dairy product allergy symptoms such as stomach discomfort, diarrhea and the like, is a dairy product which can be eaten by most people, is particularly suitable for people who are allergic to cow milk and have weak constitution, and can be used as an optimal breast milk substitute.
In recent years, the advantages of low allergenicity, high nutritional value, easy digestion and absorption, unique flavor and the like of the goat milk formula milk powder are pursued by consumers and become popular products in the dairy industry. However, since the goat milk has low yield, high raw material cost and is influenced by seasonal variation, manufacturers are driven by economic benefits, and the adulteration phenomenon of blending cow milk powder with low price and high yield into goat milk formula milk powder frequently occurs. The adulteration acts to not only harm the economic benefit of consumers, but also the added cow milk allergen threatens the health of cow milk allergy consumers.
In conclusion, it is necessary to establish a method for rapidly and conveniently detecting whether the goat milk formula milk powder is adulterated.
Many methods for identifying dairy product adulteration (such as electrophoresis, immunological techniques, liquid chromatography, PCR method based on DNA detection, ELISA method based on protein detection, etc.) have been developed to some extent to solve the above-mentioned problems, but they have various shortcomings. Gas chromatography is well-established in the food field, and various methods for extracting odorous compounds include headspace extraction methods such as Solid Phase Microextraction (SPME) and Dynamic Headspace (DHS), and solvent extraction methods such as distillation extraction (SDE) and solvent-assisted flavor evaporation (SAFE). SPME is a non-solvent based selective extraction method developed on the basis of solid phase extraction. The method enriches volatile compounds by utilizing a polymer stationary phase adsorption coating with different properties coated on the surface, has higher extraction efficiency, and is characterized by sensitivity, rapidness, direct application to GC-MS and the like, so that SPME is widely applied to the analysis fields of environment, food and the like.
Disclosure of Invention
The invention aims to provide a convenient method for detecting adulteration of goat milk formula milk powder, which can accurately judge whether milk powder is added in the goat milk formula milk powder or not, or whether the goat milk formula milk powder is impersonated without goat milk, and comprises the following steps:
A. establishment of aroma compound fingerprint spectrum library in non-adulterated goat milk formula milk powder
Analyzing the aroma compounds in the goat milk formula milk powder by using a gas chromatography by taking the aroma compounds in the goat milk formula milk powder without adulteration as a judgment basis to obtain the compositions of the aroma compounds;
B. establishment of aroma compound fingerprint spectrum library in unadulterated milk formula milk powder
Analyzing aroma compounds in various milk formula milk powder by adopting the same gas chromatography as the step A to obtain the compositions of the aroma compounds;
C. screening of characteristic aroma compounds in non-adulterated goat milk and cow milk formula milk powder
By comparing the compositions of various aroma compounds in the goat milk formula milk powder with the compositions of various aroma compounds in the cow milk formula milk powder, characteristic aroma compounds which are shared in the goat milk formula milk powder and are not contained in the cow milk formula milk powder and characteristic aroma compounds which are shared in the cow milk formula milk powder and are not contained in the goat milk formula milk powder are screened out and are respectively used as the characteristic aroma compounds in the goat milk formula milk powder and the cow milk formula milk powder;
D. discrimination of sample to be measured
Analyzing the aroma compounds in the sample to be detected by adopting the gas chromatography which is the same as the step A, B to obtain the compositions of various aroma compounds;
E. and comparing various aroma compounds in the sample to be detected with the characteristic aroma compounds in the non-adulterated goat milk and cow milk formula milk powder to determine whether the sample to be detected contains goat milk or not and whether the sample to be detected is adulterated or not.
The method of the invention establishes a fingerprint spectrum library of aroma compounds in the non-adulterated goat milk formula milk powder and a fingerprint spectrum library of aroma compounds in the non-adulterated cow milk formula milk powder, compares the measured aroma compounds in the sample to be tested with the characteristic aroma compounds in the non-adulterated goat milk and cow milk formula milk powder, and can determine whether the sample to be tested contains goat milk and whether the sample to be tested is adulterated. If the sample to be detected does not contain the goat milk, the detected sample does not contain the characteristic aroma compound in the goat milk formula milk powder; if the sample to be detected is adulterated, the characteristic aroma compounds in the goat milk formula milk powder and the characteristic aroma compounds in the cow milk formula milk powder are contained after detection, and the detection can be determined by one-time detection.
Generally, the animal milk added in the preparation process of the non-adulterated goat milk formula milk powder is goat milk only, so that the composition of various aroma compounds in the non-adulterated goat milk formula milk powder can be accurately determined in the step A; the animal milk added in the preparation process of the unadulterated cow milk formula milk powder is only cow milk, so that the composition of various aroma compounds in the unadulterated cow milk formula milk powder can be accurately determined in the step B.
The non-adulterated goat milk formula milk powder in the method is commercially available formula milk powder taking goat milk as a main raw material, such as goat milk powder 1(Y1), goat milk powder 2(Y2), goat milk powder 3(Y3), goat milk powder 4(Y4), goat milk powder 5(Y5) and goat milk powder 6 (Y6); the non-adulterated cow milk formula milk powder in the method is commercially available formula milk powder taking cow milk as a main raw material, such as cow milk powder 1(N1), cow milk powder 2(N2), cow milk powder 3(N3), cow milk powder 4(N4), cow milk powder 5(N5) and cow milk powder 6 (N6).
Preferably, the method further comprises the following steps:
1) according to the composition of various aroma compounds in the non-adulterated goat milk formula milk powder obtained in the step A, aiming at each non-adulterated goat milk formula milk powder, selecting aroma compounds which are common in the same animal milk raw materials and are specific to different animal milk raw materials as characteristic aroma compounds; and B, selecting the aroma compounds which are common in the same animal milk raw materials and are unique to different animal milk raw materials as characteristic aroma compounds for each non-adulterated cow milk formula milk powder according to the composition of the aroma compounds in the non-adulterated cow milk formula milk powder obtained in the step B. Performing orthogonal partial least squares discriminant analysis according to the content composition of the aroma compounds to obtain an orthogonal partial least squares discriminant analysis (OPLS-DA) fractional scatter diagram of various unadulterated goat milk formula milk powder and cow milk formula milk powder, and obtaining a VIP diagram based on an OPLS-DA model;
2) screening out common compounds as index aroma compounds of the non-adulterated goat milk formula milk powder by comparing the characteristic aroma compounds of the non-adulterated goat milk formula milk powder with the compounds with the VIP value larger than 1 in a VIP picture; through the comparison of the characteristic aroma compounds of the milk formula milk powder without adulteration and the compounds with the VIP value larger than 1 in the VIP picture, the common compounds are screened out to be used as the index aroma compounds of the milk formula milk powder without adulteration;
3) and D, according to the composition of the various aroma compounds in the sample to be detected obtained in the step D, comparing the aroma compounds with index compounds in milk and goat milk formula milk powder, and determining the category of the sample to be detected and whether the sample to be detected is adulterated. Performing principal component analysis on the content composition of the various aroma compounds measured in the step D to obtain a principal component analysis scatter diagram of the sample to be measured;
4) and further determining whether the sample is adulterated according to the relative position relationship between the principal component analysis scatter diagram of the sample to be detected and the principal component analysis scatter diagram of the non-adulterated goat milk formula milk powder and the principal component analysis scatter diagram of the non-adulterated cow milk formula milk powder.
In the actual operation process, if the main component analysis scatter diagram of the sample to be detected is not in the area where the main component analysis scatter diagram of the unadulterated goat milk formula milk powder is located, adulterating the sample to be detected; if the principal component analysis scatter diagram of the sample is closer to the principal component analysis scatter diagram of the milk formula without adulteration, more milk is added, and conversely, less milk is added.
The non-adulterated goat milk formula milk powder in the method is Y1, Y2, Y3, Y4, Y5 and Y6. The existing goat milk formula milk powder in the market mainly comprises main brands of Y1, Y2, Y3, Y4, Y5, Y6 and the like, and the varieties of the goat milk formula milk powder can be covered more comprehensively by selecting the goat milk formula milk powder with the brands as standards established by a standard spectrum library.
The non-adulterated cow milk formula milk powder in the method is N1, N2, N3, N4, N5 and N6. The existing milk formula milk powder in the market mainly comprises N1, N2, N3, N4, N5, N6 and the like as main brands, and the brands of milk formula milk powder are selected as standards established by a standard spectrum library, so that the types of the milk formula milk powder can be more comprehensively covered.
Preferably, the index aroma compounds of the non-adulterated goat milk formula milk powder are as follows: 2-methylbutanal, trans-2, 4-decadienol and heptyl formate. The content of the aroma compounds in different goat milk formula milk powders has certain difference, and the aroma compounds which are shared in the 3 goat milk formula milk powders and are not contained in the cow milk formula milk powder are selected as index aroma compounds, so that the existing goat milk formula milk powders can be more comprehensively covered, and a more direct, clear and objective detection standard is provided for detection.
Preferably, the non-adulterated cow milk formula has the following index compounds: 1-octen-3-ol, trans-2-octenal and trans, trans-3, 5-dioctenone. The content of aroma compounds in different milk formula milk powder has certain difference, and the aroma compounds which are shared in the milk formula milk powder 3 and are not contained in the goat milk formula milk powder are selected as index aroma compounds, so that the existing milk formula milk powder can be more comprehensively covered, and a more direct, clear and objective detection standard is provided for detection.
Preferably, the aroma extraction method comprises:
selecting Solid Phase Micro Extraction (SPME)
Preparing milk powder hydrolysate (0.5g/mL) according to the formula milk powder mixing method, weighing 3mL of sample in a 10mL solid phase microextraction headspace bottle, placing in a 55 ℃ constant temperature water bath, balancing for 20min, inserting an extraction head of fiber coating CAR/DVB/PDMS (65 μm) into the headspace bottle, and adsorbing for 40 min.
The preferable conditions of the gas chromatography detection are as follows:
volatile compounds are separated on a polar chromatographic column DB-WAX and a non-polar chromatographic column DB-5 to achieve mutual evidence of double columns; the carrier gas is helium; separating the compound on a chromatographic column by adopting a gradient heating mode, and using a mass spectrum detector; the constant flow rate is 1.2 mL/min; the injection port temperature is 250 ℃, and the pressure is 14.87 psi; the shunt ratio is set to the no-shunt mode.
The preferred gradient temperature increasing program is as follows:
the initial temperature is 40 ℃, and the temperature is kept for 3 min;
then heating to 150 ℃ at the heating rate of 5 ℃/min;
then heating to 210 ℃ at the heating rate of 4 ℃/min;
finally, the temperature is increased to 250 ℃ at the speed of 5 ℃/min and kept for 3 min.
By adopting the gas chromatography condition and the method, the aroma compounds in various formulas can be detected more accurately and rapidly.
Preferably, the mass spectrometry parameters are as follows:
the ion source temperature was set at 230 ℃, the transmission line temperature was set at 250 ℃, the quadrupole rod temperature was set at 150 ℃, the Electron Impact (EI) ion source, the electron energy was 70eV, the mass scan range m/z was set at 29-500, and the solvent delay was set at 4 min.
The method has the following beneficial effects:
1) the method can determine the type of the formula milk powder to which the sample to be detected belongs by establishing the fingerprint spectrum library of the aroma compounds of different types of formula milk powder, and further determine whether the formula milk powder is adulterated according to the composition of the index aroma compounds. Furthermore, the auxiliary principal component analysis method can judge whether adulteration is carried out or not more intuitively and can preliminarily judge the addition amount. The method can firstly determine whether the formula milk powder contains the goat milk (after detection, the formula milk powder contains the index compounds in 3-5 goat milk formula milk powders) according to the types of the index aroma compounds, and can also judge the condition that the goat milk formula milk powder is directly added into the goat milk formula milk powder.
2) The method has low detection limit, and can detect 5 percent or more of adulteration of the milk;
3) the method has the advantages of simple steps, convenient operation, visual result and wide popularization and application prospect.
Drawings
FIG. 1 shows a waterfall plot of a goat milk formula milk powder without adulteration;
FIG. 2 shows a waterfall plot of milk formula without adulteration;
FIG. 3 is a OPLS-DA fractional scatter plot of non-adulterated cow's milk and goat's milk formula;
FIG. 4 is a VIP graph of an unadulterated cow's milk and goat's milk formula;
FIG. 5 is a scatter plot of principal component analysis of goat milk formula containing varying proportions of milk adulterated with goat milk;
FIG. 6 is a scatter plot of principal component analysis of goat milk formula containing different varieties of milk adulterated with goat milk;
FIG. 7 is a scatter plot of principal component analysis of different goat milk formulas containing the same cow milk adulterated.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
The embodiment relates to an effective identification method of goat milk formula milk powder adulterated with cow milk, and mainly relates to the establishment of a fingerprint spectrum library, an OPLS-DA score scatter diagram and a VIP diagram of aroma compounds in non-adulterated goat milk and cow milk formula milk powder, and the establishment of index aroma compounds.
1. Establishment of aroma compound fingerprint spectrum library in formula milk powder without adulterated goat milk and cow milk
(1) Taking Y1, Y2, Y3, Y4, Y5 and Y6 as standard products of the non-adulterated goat milk formula milk powder; n1, N2, N3, N4, N5 and N6 are used as standard substances of the unadulterated milk formula milk powder.
(2) Treatment of materials
Weighing 0.6g sheep milk and cow milk formula milk powder, dissolving in water, and diluting to 4ml to obtain formula milk powder hydrolysate.
(3) Reagent and apparatus
N-hexane was purchased from Thermo Fisher, usa, and chromatographically pure; n-alkanes (C7-C30) and 2-methyl-3-heptanone were purchased from Sigma, USA, chromatographically pure; helium (99.999% pure) and nitrogen (99.9%) pure were purchased from helium pebei gas industries, ltd, beijing. Gas Chromatograph (GC) model 7890 and 7000B triple quadrupole mass spectra, both available from Agilent, usa.
(4) Gas chromatography detection
Chromatographic parameters: the chromatographic columns are polar chromatographic column DB-WAX (30m × 0.25mm × 0.25 μm) and nonpolar chromatographic column DB-5ms (30m × 0.25mm × 0.25 μm); the carrier gas is helium; the separation of the compound on the chromatographic column is realized by adopting a gradient temperature rise mode, and the gradient program comprises the following steps: the initial temperature is 40 ℃, and the temperature is kept for 3 min; then heating to 150 ℃ at the heating rate of 5 ℃/min; then heating to 210 ℃ at the heating rate of 4 ℃/min; finally, the temperature is increased to 250 ℃ at the speed of 5 ℃/min and kept for 3 min. Using a mass spectrometer; the constant flow rate is 1.2 mL/min; the injection port temperature was 250 ℃ and the pressure was 14.87 psi.
Mass spectrum parameters: the ion source temperature was set at 230 ℃, the transmission line temperature was set at 250 ℃, the quadrupole rod temperature was set at 150 ℃, the electron bombarded the ion source, the electron energy was 70eV, the mass scan range m/z was set at 29-500, and the solvent delay was set at 4 min.
(5) Data analysis
Characterization of aroma compounds: and identifying the aroma compounds extracted from different samples by adopting a mode of combining mass spectrometry and standard compound Retention Index (RI) comparison.
Firstly, matching and identifying mass spectrum spectrogram of an object to be detected and mass spectrum structure information of a standard compound in an NIST14 spectrum library in mass spectrum characterization, and performing primary screening on the compound with the matching degree of more than or equal to 800;
secondly, the RI values of the target compound and the standard compound are compared under the same GC-O-MS parameter condition, and the target compound is further characterized. The RI value of the target compound is calculated as follows:
wherein, t in the formulaaRepresents the retention time of compound a in the sample; t is tnNormal paraffin standard C representing n carbon atomnThe retention time of (c); retention time t of sample aaTwo normal alkanes adjacent to each othernAnd Cn+1Between the retention times of (c).
And finally, integrating the results of the qualitative mode to obtain the final identification result of the volatile compound.
Quantification of aroma compounds:
the quantitative analysis adopts an internal standard semi-quantitative method, the GC-MS adopts 2-methyl-3-heptanone with the concentration of 0.816 mu g/mu L as an internal standard compound under a SCAN mode, and the quantitative analysis is carried out on the target compound in the sample by calculating the relationship between the peak area and the concentration, and the formula is as follows:
wherein, Ca、CisRespectively representing the concentrations of the target compound a and the internal standard compound; a. thea、AisThe peak areas of the target compound and the internal standard compound are respectively expressed.
(7) Establishment of fingerprint atlas database
Fig. 1 and 2 are waterfall plots of non-adulterated goat milk and cow milk formula milk powder, respectively, and qualitative analysis can be performed through mass spectrum data and RI comparison standards, and quantitative analysis can be performed through peak areas. Table 1 shows the composition of aroma compounds of various formulas without blending pseudo goat milk; table 2 shows the composition of aroma compounds of various milk formula without adulteration, each raw material was processed in parallel for three times. By comparing aroma compounds in the goat milk formula milk powder without adulteration with aroma compounds in the cow milk formula milk powder, 2-furancarbinol, 2-methylbutanal, 2, 3-pentanedione, trans-2, 4-decadienol and heptyl formate are the unique aroma compounds in the goat milk formula milk powder; 1-octen-3-ol, trans-2-octenal, acetophenone and trans, trans-3, 5-dioctyl ketene are peculiar aroma compounds in milk formula milk powder.
2. Establishment of OPLS-DA (Oplops-data acquisition) score scatter diagram and VIP (very important person) diagram
And the data in the table 1 and the table 2 are subjected to OPLS-DA analysis through Simca-P +14.1 data processing software, the OPLS-DA with a supervision function can strengthen the separation between the groups to be observed, and the characteristic mark of the sample difference can be determined while the difference between the two groups is distinguished. The aroma compounds of the goat milk and cow milk formula milk powder were analyzed by using OPLS-DA, as shown in FIG. 3, the two samples clustered well on the OPLS-DA score chart, R2X-99.88%, the selected component can characterize 99.88% change in the dataset.
Meanwhile, based on the OPLS-DA model, a VIP map can be obtained (fig. 4). VIP indicates the importance of the variable in making the difference between groups, and variable X is significantly different between groups when VIP > 1.0.
Determination of index aroma compounds in formula milk powder without adulterated goat milk and cow milk
By comparing the specific aroma compounds of the sheep milk and cow milk formula in the step (7) with the aroma compounds in the sheep milk and cow milk formula in the figure 4, trans-2, 4-decadienol, 2-methylbutyraldehyde and heptyl formate can be used as index compounds in the sheep milk formula; trans-2-octenal, 1-octen-3-ol and trans, trans-3, 5-dioctyl ketene can be used as index aroma compounds in milk formula milk powder.
Example 2
The embodiment relates to the discrimination of adulterated milk powder mixed with different proportions of cow milk formula milk powder in goat milk formula milk powder, which mainly carries out the comparison of index aroma compounds in the adulterated milk powder and non-adulterated goat milk and cow milk formula milk powder and the Principal Component Analysis (PCA) of adulterated samples.
1) The detection of the adulterated sample takes the non-adulterated goat milk formula milk powder in the embodiment 1 as a base substance, and replaces the same weight of the non-adulterated goat milk formula milk powder with 5%, 10%, 20%, 40% and 80% of the total weight of the non-adulterated goat milk formula milk powder, thereby simulating the goat milk adulterated milk powder artificially added with the goat milk formula milk powder. The sample treatment and data analysis methods were the same as in example 1, and the compositions of the indicative aroma compounds in the samples of this example obtained are shown in table 3. Further proves that in the actual detection process, whether the goat milk formula milk powder is adulterated or not is accurately determined by detecting the index aroma compound, and the lowest detection limit of the method can be 5%.
2) Conducting a PCA analysis on said sample
The main component analysis of the aroma compounds in the sample of this example was performed using Simca-P +14.1 data processing software to obtain a main component analysis scattergram of FIG. 5.● is non-adulterated goat milk formula milk powder (Y); ■ is milk formula (N) without adulteration; the tangle-solidup is the adulterated goat milk formula milk powder (C) which is added into the milk formula milk powder. The main component scatter diagram shows that the adulterated goat milk formula milk powder doped with cow milk formula milk powder is different from the non-adulterated goat milk formula milk powder. And the more the blended milk formula milk powder is, the farther the point is from the unadulterated goat milk formula milk powder through the auxiliary line connecting the two areas of the adulterated goat milk formula milk powder and the unadulterated goat milk formula milk powder. The adulterated formula milk powder can be visually and rapidly seen through the scatter diagram.
TABLE 3 composition of indicative aroma compounds in goat milk formula milk powder with different milk adulteration ratios
C: goat milk formula milk powder blended with cow milk formula milk powder
Example 3
The embodiment relates to the discrimination of adulteration of different types of milk formula milk powder respectively mixed in goat milk formula milk powder, the comparison of index aroma compounds in main adulterated milk powder and non-adulterated goat milk and milk formula milk powder and the PCA analysis of adulterated samples.
1) The detection of the adulterated sample takes the non-adulterated goat milk formula milk powder in the embodiment 1 as a base substrate, and different varieties of cow milk formula milk powder with the total weight of 5 percent respectively replace the same weight of the non-adulterated goat milk formula milk powder, so that the goat milk adulterated milk powder artificially added with the cow milk formula milk powder is simulated. The sample treatment and data analysis methods were the same as in example 1, and the compositions of the indicative aroma compounds in the samples of this example obtained are shown in table 4. Whether the goat milk formula milk powder is adulterated or not is determined accurately by detecting the index aroma compounds, and the influence of the adulteration of different types of cow milk formula milk powder on the lowest detection limit can be verified.
2) Conducting a PCA analysis on said sample
The aroma compounds in this example were subjected to principal component analysis using Simca-P +14.1 data processing software. A principal component analysis scattergram of fig. 6 was obtained. ● is non-adulterated goat milk formula milk powder (Y); ■ is milk formula (N) without adulteration; the tangle-solidup is the adulterated goat milk formula milk powder (C) which is added into the milk formula milk powder. The main component scatter diagram shows that the adulterated goat milk formula milk powder doped with cow milk formula milk powder is different from the non-adulterated goat milk formula milk powder. And the adulterated formula milk powder can be visually and rapidly seen through the scatter diagram. The influence of the milk formula milk powder variety on the minimum detection limit is eliminated when the minimum detection limit is set to be 5 percent.
TABLE 4 composition of indicative aroma compounds in goat milk formula milk powder with adulterated cow's milk of different varieties
C: goat milk formula milk powder blended with cow milk formula milk powder
Example 4
The embodiment relates to a method for judging adulteration of random cow milk formula milk powder mixed into 6 goat milk formula milk powders respectively, which mainly comprises the steps of comparing the adulterated milk powder with index aroma compounds in non-adulterated goat milk formula milk powder and main component analysis (PCA) of adulterated samples.
1) The detection of the adulterated sample takes 6 non-adulterated goat milk formula milk powders in example 1 as a substrate, and cow milk formula milk powders (random ones) accounting for 20 percent of the total weight replace the non-adulterated goat milk formula milk powders with the same weight respectively, so that the goat milk adulterated milk powders artificially added with the cow milk formula milk powders are simulated. Sample treatment and data analysis were performed in the same manner as in example 1, and the compositions of the index aroma compounds in the samples of this example obtained are shown in Table 5. Further proves that in the actual detection process, the accuracy of determining whether the goat milk formula milk powder is adulterated or not and the detection range of the goat milk formula milk powder is verified by detecting the index aroma compounds.
2) Conducting a PCA analysis on said sample
The aroma compounds in the samples of this example were analyzed for their major components using Simca-P +14.1 data processing software. A principal component analysis scattergram of fig. 7 was obtained. ● is non-adulterated goat milk formula milk powder (Y); ■ is milk formula (N) without adulteration; the tangle-solidup is the adulterated goat milk formula milk powder (C) which is added into the milk formula milk powder. The main component scatter diagram shows that various adulterated goat milk formula milk powder doped with cow milk formula milk powder is different from non-adulterated goat milk formula milk powder. And the adulterated goat milk formula milk powder is gathered together, and the non-adulterated goat milk formula milk powder is gathered together. Further proves that the method has wide detectable range.
TABLE 5 composition of indicative aroma compounds in different goat milk formula milk powder with same cow milk adulterated
C: goat milk formula milk powder blended with cow milk formula milk powder
In conclusion, whether the formula milk powder sold in the market is adulterated or not can be determined by observing the composition of the aroma compounds of the formula milk powder, and the adulterated formula milk powder and the non-adulterated formula milk powder can be more intuitively and quickly identified by further bringing a sample into a model through principal component analysis.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A convenient method for detecting adulteration of goat milk formula milk powder is characterized by comprising the following steps:
A. establishment of aroma compound fingerprint spectrum library in non-adulterated goat milk formula milk powder
Analyzing aroma compounds in the non-adulterated goat milk formula milk powder by using a gas chromatography to obtain the composition of the aroma compounds;
B. establishment of aroma compound fingerprint spectrum library in unadulterated milk formula milk powder
Analyzing the aroma compounds in various milk formula milk powder by adopting the same gas chromatography as the step A to obtain the compositions of the aroma compounds;
C. screening of characteristic aroma compounds in non-adulterated goat milk and cow milk formula milk powder
By comparing the compositions of various aroma compounds in the goat milk formula milk powder with the compositions of various aroma compounds in the cow milk formula milk powder, characteristic aroma compounds which are shared in the goat milk formula milk powder and are not contained in the cow milk formula milk powder and characteristic aroma compounds which are shared in the cow milk formula milk powder and are not contained in the goat milk formula milk powder are screened out and respectively used as the characteristic aroma compounds in the goat milk and the cow milk formula milk powder;
D. discrimination of sample to be measured
Analyzing the aroma compounds in the sample to be detected by adopting the gas chromatography which is the same as the step A, B to obtain the compositions of various aroma compounds;
E. and comparing the ratio of the aroma compounds in the sample to be detected with the characteristic aroma compounds in the non-adulterated goat milk and cow milk formula milk powder, determining whether the sample to be detected contains goat milk or not, and determining whether the sample to be detected is adulterated or not.
2. The method of claim 1, further comprising the steps of:
1) according to the composition of various aroma compounds in the non-adulterated goat milk formula milk powder obtained in the step A, aiming at each non-adulterated goat milk formula milk powder, selecting aroma compounds which are common in the same animal milk raw materials and are specific to different animal milk raw materials as characteristic aroma compounds; and B, selecting the aroma compounds which are common in the same animal milk raw materials and are unique to different animal milk raw materials as characteristic aroma compounds for each non-adulterated cow milk formula milk powder according to the composition of the aroma compounds in the non-adulterated cow milk formula milk powder obtained in the step B. Performing partial least squares discriminant analysis according to the content composition of the aroma compounds to obtain partial least squares discriminant analysis (OPLS-DA) fractional scattergrams of various unadulterated goat milk formula milk powder and cow milk formula milk powder, and obtaining a VIP map based on an OPLS-DA model;
2) screening out common compounds as index aroma compounds of the non-adulterated goat milk formula milk powder by comparing the characteristic aroma compounds of the non-adulterated goat milk formula milk powder with the compounds with the VIP value larger than 1 in a VIP picture; through the comparison of the characteristic aroma compounds of the milk formula milk powder without adulteration and the compounds with the VIP value larger than 1 in the VIP picture, the common compounds are screened out to be used as the index aroma compounds of the milk formula milk powder without adulteration;
3) and D, according to the composition of the various aroma compounds in the sample to be detected obtained in the step D, comparing the aroma compounds with index compounds in milk and goat milk formula milk powder, and determining the category of the sample to be detected and whether the sample to be detected is adulterated. Performing principal component analysis on the content composition of the various aroma compounds measured in the step D to obtain a principal component analysis scatter diagram of the sample to be measured;
4) and further determining whether the sample is adulterated according to the relative position relationship between the principal component analysis scatter diagram of the sample to be detected and the principal component analysis scatter diagram of the non-adulterated goat milk formula milk powder and the principal component analysis scatter diagram of the non-adulterated cow milk formula milk powder.
3. The method as claimed in claim 1 or 2, wherein the non-adulterated goat milk formula is a goat milk formula of major brands such as Y1, Y2, Y3, Y4, Y5 and Y6.
4. The method according to claim 1 or 2, wherein the unadulterated milk formula is a milk formula with major brands N1, N2, N3, N4, N5 and N6.
5. The method according to claims 1-3, wherein the unadulterated goat milk formula has the following indicative aroma compounds: 2-methylbutanal, trans-2, 4-decadienal and heptyl formate.
6. The method according to claims 1, 2 and 4, wherein the non-adulterated milk formula has the following indicative compounds: 1-octen-3-ol, trans-2-octenal and trans, trans-3, 5-dioctenone.
7. The method according to claims 1-6, characterized in that the aroma extraction method is Solid Phase Microextraction (SPME) under the conditions that the sample is put into a thermostat water bath at 55 ℃ and equilibrated for 20min, and then inserted into a headspace bottle for 40min with an extraction head of fiber coating CAR/DVB/PDMS (65 μm).
8. The method according to claim 1, wherein the gas chromatography detection conditions are: the gas chromatographic column is a polar chromatographic column DB-WAX and a nonpolar chromatographic column DB-5 ms; the carrier gas is helium; separating the compound on a chromatographic column by adopting a gradient heating mode, and using a mass spectrum detector; the constant flow rate is 1.2 mL/min; the injection port temperature is 250 ℃, and the pressure is 14.87 psi; the shunt ratio is set to the no-shunt mode.
9. The method according to claims 1 and 9, characterized in that the gradient ramp-up procedure is: the initial temperature is 40 ℃, and the temperature is kept for 3 min; then heating to 150 ℃ at the heating rate of 5 ℃/min; then heating to 210 ℃ at the heating rate of 4 ℃/min; finally, the temperature is increased to 250 ℃ at the speed of 5 ℃/min and kept for 3 min.
10. The method of claims 1 and 10, wherein the mass spectrometry conditions are: the ion source temperature was set at 230 ℃, the transmission line temperature was set at 250 ℃, the quadrupole rod temperature was set at 150 ℃, the Electron Impact (EI) ion source, the electron energy was 70eV, the mass scan range m/z was set at 29-500, and the solvent delay was set at 4 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011573090.5A CN112578053A (en) | 2020-12-28 | 2020-12-28 | Method for judging adulteration of goat milk formula milk powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011573090.5A CN112578053A (en) | 2020-12-28 | 2020-12-28 | Method for judging adulteration of goat milk formula milk powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112578053A true CN112578053A (en) | 2021-03-30 |
Family
ID=75139975
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011573090.5A Pending CN112578053A (en) | 2020-12-28 | 2020-12-28 | Method for judging adulteration of goat milk formula milk powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112578053A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114354814A (en) * | 2022-01-13 | 2022-04-15 | 青岛农业大学 | Small molecular marker for detecting adulterated cow milk in goat milk product |
| CN116046956A (en) * | 2023-02-24 | 2023-05-02 | 北京三元食品股份有限公司 | Analysis and identification method for infant formula milk powder with different milk-based components |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101271107A (en) * | 2008-04-09 | 2008-09-24 | 陕西科技大学 | Fast immunology detecting method for goat milk and its milk product doped with cow's milk |
| CN105021736A (en) * | 2015-08-04 | 2015-11-04 | 内蒙古农业大学 | Authenticity identifying method and system for raw milk or liquid milk |
| CN106011242A (en) * | 2016-05-26 | 2016-10-12 | 陕西师范大学 | Extensive and accurate quantitative detection method for milk component in goat milk powder |
| CN106749598A (en) * | 2016-11-30 | 2017-05-31 | 杭州帕匹德科技有限公司 | A kind of feature peptide for detecting the adulterated ratio of milk powder in goat milk powder is combined and method |
| CN110221007A (en) * | 2019-06-04 | 2019-09-10 | 广西壮族自治区水牛研究所 | Adulterated detection method in a kind of identification buffalo's milk |
| CN110487878A (en) * | 2019-08-16 | 2019-11-22 | 陕西科技大学 | A kind of adulterated determination method of wide spectrum of fresh sheep cream |
-
2020
- 2020-12-28 CN CN202011573090.5A patent/CN112578053A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101271107A (en) * | 2008-04-09 | 2008-09-24 | 陕西科技大学 | Fast immunology detecting method for goat milk and its milk product doped with cow's milk |
| CN105021736A (en) * | 2015-08-04 | 2015-11-04 | 内蒙古农业大学 | Authenticity identifying method and system for raw milk or liquid milk |
| CN106011242A (en) * | 2016-05-26 | 2016-10-12 | 陕西师范大学 | Extensive and accurate quantitative detection method for milk component in goat milk powder |
| CN106749598A (en) * | 2016-11-30 | 2017-05-31 | 杭州帕匹德科技有限公司 | A kind of feature peptide for detecting the adulterated ratio of milk powder in goat milk powder is combined and method |
| CN110221007A (en) * | 2019-06-04 | 2019-09-10 | 广西壮族自治区水牛研究所 | Adulterated detection method in a kind of identification buffalo's milk |
| CN110487878A (en) * | 2019-08-16 | 2019-11-22 | 陕西科技大学 | A kind of adulterated determination method of wide spectrum of fresh sheep cream |
Non-Patent Citations (1)
| Title |
|---|
| 田怀香等: "指纹图谱技术在生鲜乳掺假检测中的研究进展", 《食品安全质量检测学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114354814A (en) * | 2022-01-13 | 2022-04-15 | 青岛农业大学 | Small molecular marker for detecting adulterated cow milk in goat milk product |
| CN116046956A (en) * | 2023-02-24 | 2023-05-02 | 北京三元食品股份有限公司 | Analysis and identification method for infant formula milk powder with different milk-based components |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ogrinc et al. | The application of NMR and MS methods for detection of adulteration of wine, fruit juices, and olive oil. A review | |
| CN112578053A (en) | Method for judging adulteration of goat milk formula milk powder | |
| Zhang et al. | Volatile fingerprints and biomarkers of three representative kiwifruit cultivars obtained by headspace solid-phase microextraction gas chromatography mass spectrometry and chemometrics | |
| CN104316635A (en) | Method for rapidly identifying flavor and quality of fruits | |
| CN108426968B (en) | Classification method of winter honey and Chinese tallow tree honey | |
| CN107782827B (en) | Cheese characteristic flavor substance analysis method and fingerprint spectrum thereof | |
| CN107478736A (en) | A kind of method that hops freshness is judged based on volatile ingredient composition | |
| Park et al. | Analysis of ethanol in soy sauce using electronic nose for halal food certification | |
| Kadar et al. | Gas chromatography coupled with mass spectrometry-based metabolomics for the classification of tempe from different regions and production processes in Indonesia | |
| CN107389813A (en) | Rascal, dried orange peel, the dried immature fruit of citron orange and the method for Fructus Aurantii are differentiated based on chemical classification and UPLC Tof MS | |
| CN106770796A (en) | The method that static headspace-GC-MS combination determines ready-mixed oil harmonic proportion | |
| CN104132905A (en) | Detection method for adulterated sesame oil | |
| CN116482284A (en) | Human milk characteristic fatty acid fingerprint and application thereof in authenticity identification | |
| CN109781893A (en) | A kind of method of Rapid identification red date slices quality and processing method | |
| CN101509901B (en) | Method for analyzing origin of amino acid in brewed sauce | |
| CN111738548A (en) | Jasmine tea aroma quality evaluation method and application thereof | |
| CN106324127B (en) | The pueraria root powder true and false identifies and the method for maca assay | |
| CN113820434B (en) | Method for identifying maturity of acacia honey | |
| CN114200055B (en) | Method for rapidly identifying raw sugarcane juice brown sugar and brown granulated sugar based on characteristic aroma substance GC-IMS fingerprint | |
| US10119947B2 (en) | Protein-rich microalgal biomass compositions of optimized sensory quality | |
| CN116046956A (en) | Analysis and identification method for infant formula milk powder with different milk-based components | |
| CN110887921A (en) | Method for efficiently and rapidly analyzing characteristic volatile components of eucommia leaves and fermentation product thereof | |
| Kolenc et al. | Determination of Camelina Oil Sterol Composition and Its Application for Authenticity Studies. | |
| CN112595784B (en) | Method for distinguishing Chinese bee honey and Italian bee honey | |
| CN114062568A (en) | Method for identifying variety of cherry by GC-IMS technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210330 |
|
| RJ01 | Rejection of invention patent application after publication |