CN114019050B - Method for detecting mixing of peanut oil into edible oil based on volatile components - Google Patents
Method for detecting mixing of peanut oil into edible oil based on volatile components Download PDFInfo
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- 235000019483 Peanut oil Nutrition 0.000 title claims abstract description 87
- 239000000312 peanut oil Substances 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000008157 edible vegetable oil Substances 0.000 title claims abstract description 21
- 238000002156 mixing Methods 0.000 title description 9
- WHMWOHBXYIZFPF-UHFFFAOYSA-N 2-ethyl-3,(5 or 6)-dimethylpyrazine Chemical compound CCC1=NC(C)=CN=C1C WHMWOHBXYIZFPF-UHFFFAOYSA-N 0.000 claims abstract description 32
- DTUQWGWMVIHBKE-UHFFFAOYSA-N phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 18
- 239000001363 2-ethyl-3,5-dimethylpyrazine Substances 0.000 claims abstract description 16
- YOMSJEATGXXYPX-UHFFFAOYSA-N 2-methoxy-4-vinylphenol Chemical compound COC1=CC(C=C)=CC=C1O YOMSJEATGXXYPX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229940100595 phenylacetaldehyde Drugs 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 13
- XYYMFUCZDNNGFS-UHFFFAOYSA-N 2-methylheptan-3-one Chemical compound CCCCC(=O)C(C)C XYYMFUCZDNNGFS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010348 incorporation Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 48
- 239000003921 oil Substances 0.000 claims description 32
- 235000019198 oils Nutrition 0.000 claims description 32
- 238000000605 extraction Methods 0.000 claims description 23
- 239000010495 camellia oil Substances 0.000 claims description 19
- 239000012224 working solution Substances 0.000 claims description 17
- 239000012488 sample solution Substances 0.000 claims description 15
- 230000000630 rising effect Effects 0.000 claims description 12
- 238000012417 linear regression Methods 0.000 claims description 11
- 235000019484 Rapeseed oil Nutrition 0.000 claims description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 10
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 10
- 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 10
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims description 10
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 10
- 238000002470 solid-phase micro-extraction Methods 0.000 claims description 8
- 239000002199 base oil Substances 0.000 claims description 7
- 239000008159 sesame oil Substances 0.000 claims description 7
- 235000011803 sesame oil Nutrition 0.000 claims description 7
- 239000003549 soybean oil Substances 0.000 claims description 7
- 235000012424 soybean oil Nutrition 0.000 claims description 7
- 235000020238 sunflower seed Nutrition 0.000 claims description 7
- 240000007594 Oryza sativa Species 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 6
- 235000009566 rice Nutrition 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
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- 238000001819 mass spectrum Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
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- 235000017060 Arachis glabrata Nutrition 0.000 description 3
- 244000105624 Arachis hypogaea Species 0.000 description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 description 3
- 235000018262 Arachis monticola Nutrition 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000020232 peanut Nutrition 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
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- 238000001319 headspace solid-phase micro-extraction Methods 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
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- 235000008390 olive oil Nutrition 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- KZJWDPNRJALLNS-VPUBHVLGSA-N (-)-beta-Sitosterol Natural products O[C@@H]1CC=2[C@@](C)([C@@H]3[C@H]([C@H]4[C@@](C)([C@H]([C@H](CC[C@@H](C(C)C)CC)C)CC4)CC3)CC=2)CC1 KZJWDPNRJALLNS-VPUBHVLGSA-N 0.000 description 1
- CSVWWLUMXNHWSU-UHFFFAOYSA-N (22E)-(24xi)-24-ethyl-5alpha-cholest-22-en-3beta-ol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(CC)C(C)C)C1(C)CC2 CSVWWLUMXNHWSU-UHFFFAOYSA-N 0.000 description 1
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 1
- KLEXDBGYSOIREE-UHFFFAOYSA-N 24xi-n-propylcholesterol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CCC)C(C)C)C1(C)CC2 KLEXDBGYSOIREE-UHFFFAOYSA-N 0.000 description 1
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 1
- 235000019737 Animal fat Nutrition 0.000 description 1
- LPZCCMIISIBREI-MTFRKTCUSA-N Citrostadienol Natural products CC=C(CC[C@@H](C)[C@H]1CC[C@H]2C3=CC[C@H]4[C@H](C)[C@@H](O)CC[C@]4(C)[C@H]3CC[C@]12C)C(C)C LPZCCMIISIBREI-MTFRKTCUSA-N 0.000 description 1
- ARVGMISWLZPBCH-UHFFFAOYSA-N Dehydro-beta-sitosterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)CCC(CC)C(C)C)CCC33)C)C3=CC=C21 ARVGMISWLZPBCH-UHFFFAOYSA-N 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- HZYXFRGVBOPPNZ-UHFFFAOYSA-N UNPD88870 Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)=CCC(CC)C(C)C)C1(C)CC2 HZYXFRGVBOPPNZ-UHFFFAOYSA-N 0.000 description 1
- MJVXAPPOFPTTCA-UHFFFAOYSA-N beta-Sistosterol Natural products CCC(CCC(C)C1CCC2C3CC=C4C(C)C(O)CCC4(C)C3CCC12C)C(C)C MJVXAPPOFPTTCA-UHFFFAOYSA-N 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- -1 for example Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000021281 monounsaturated fatty acids Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 235000002378 plant sterols Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 235000015500 sitosterol Nutrition 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- NLQLSVXGSXCXFE-UHFFFAOYSA-N sitosterol Natural products CC=C(/CCC(C)C1CC2C3=CCC4C(C)C(O)CCC4(C)C3CCC2(C)C1)C(C)C NLQLSVXGSXCXFE-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- HCXVJBMSMIARIN-PHZDYDNGSA-N stigmasterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)/C=C/[C@@H](CC)C(C)C)[C@@]1(C)CC2 HCXVJBMSMIARIN-PHZDYDNGSA-N 0.000 description 1
- 235000016831 stigmasterol Nutrition 0.000 description 1
- 229940032091 stigmasterol Drugs 0.000 description 1
- BFDNMXAIBMJLBB-UHFFFAOYSA-N stigmasterol Natural products CCC(C=CC(C)C1CCCC2C3CC=C4CC(O)CCC4(C)C3CCC12C)C(C)C BFDNMXAIBMJLBB-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- 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
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Edible Oils And Fats (AREA)
Abstract
The invention provides a method for detecting the incorporation of peanut oil into edible oil based on volatile components, which takes 2-methyl-3-heptanone as an internal standard, quantitatively detects characteristic volatile components of phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol in a sample through SPME-GC/MS, calculates the ratio of peak area corresponding to the separated components of phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol to the internal standard peak area, calculates the content of the incorporated peanut oil in the sample through a standard curve, and realizes quantitative detection of the peanut oil content in the sample. The method has the advantages of good reliability, simplicity, convenience, rapidness and the like, and can relatively accurately analyze the relative content of peanut oil in edible vegetable oil and judge whether the edible vegetable oil is adulterated.
Description
Technical Field
The invention relates to the technical field of edible oil adulteration detection, in particular to a method for detecting the adulteration of peanut oil in edible oil based on volatile components.
Background
The edible vegetable oil is edible oil prepared from vegetable oil seeds, including soybean oil, rapeseed oil, sesame oil, sunflower seed oil, olive oil, tea oil, etc. The vegetable oil has a higher proportion of unsaturated fatty acids than saturated fatty acids in animal fat and oil, and contains no cholesterol, but contains beneficial plant sterols such as stigmasterol, sitosterol and the like, so that the vegetable oil is favored by people.
GB 2716-2018 describes that other grease should not be mixed in single-variety edible food oil, and if the edible vegetable blend oil is edible vegetable blend oil, the label mark should be marked with the proportion of various vegetable oils, and the processing technology should be marked on the label or the accompanying file. However, because of the different nutritional values of different vegetable oil types, the different oil processing modes result in a great difference in price of edible vegetable oil, for example, vegetable oil such as tea oil, olive oil and the like is generally high in price, and some illegal merchants are striving to obtain violence by adding cheap oil to the high-price vegetable oil. The identification of adulterated vegetable oil is important to protect the rights of consumers and legal operators.
However, as the blending mode of the vegetable oil is complex and the difference between different vegetable oils is small, the difference among the similar oils is large due to factors such as production places, production modes, varieties and the like, the complex blending problem is difficult to detect through common indexes such as fatty acid and the like, and at present, no general technical method for judging the blending of the edible vegetable oil exists.
The peanut oil is rich in nutrition, the monounsaturated fatty acid is higher than other vegetable oil, and consumers select the peanut oil, so that the unique flavor component of the peanut oil brings pleasant sensory experience to consumers, the cooking flavor is improved, and China is the largest peanut oil production and consumption country in the world. In GB/T5539-2008 qualitative test of grain and oil test grease, the peanut oil is detected by using a low-temperature water bath after saponification, and whether the peanut oil exists is judged according to the temperature when turbidity occurs. The freezing point of peanut oil is used for judging whether other grease is mixed with peanut oil or not, but the total palm oil and animal grease are easy to solidify at low temperature, and false positive is easy to occur in the method. Therefore, development of a peanut oil adulteration detection method which is simple and convenient to operate and high in accuracy is imperative.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a method for detecting the doping of the peanut oil into the edible vegetable oil based on the volatile components, which is simple and convenient to operate and high in accuracy, wherein the characteristic volatile components screened out by heat treatment (80 ℃) are used for identifying the fake, and the fake doping amount of the peanut oil can be quantitatively detected so as to meet the detection requirement of the doping of the peanut oil into the edible vegetable oil.
In order to achieve the above object, the technical scheme of the present invention is as follows.
A method for detecting the content of peanut oil in edible oil based on volatile components includes such steps as quantitatively detecting the characteristic volatile components of phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol in sample by SPME-GC/MS, calculating the ratio of peak area to internal standard peak area of the separators of phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol, and calculating the content of peanut oil in sample by standard curve.
Further, the method comprises the steps of:
s1, preparing a sample solution
Adding 2-methyl-3-heptanone serving as an internal standard into a sample to be detected to prepare a sample solution;
s2, standard working solution preparation
Peanut oil is added into base oil, and 2-methyl-3-heptanone is used as an internal standard to prepare a series of standard working solutions with the mass percent of 1% -100%;
s3, SPME-GC/MS quantitative detection
The extraction head adopting SPME method is used for respectively adsorbing the sample solution of S1 and the serial standard working solution of S2, analyzing the extraction head adsorbing volatile components by GC/MS and quantifying the volatile components, and then calculating the peak area C of the separated phenylacetaldehyde 1 Peak area C of isolate 3-ethyl-2, 5-dimethylpyrazine 2 Peak area C of isolate 4-vinyl-2-methoxyphenol 3 And internal standard peak area C 0 Ratio C of (2) 1 /C 0 、C 2 /C 0 、C 3 /C 0 ；
S4, drawing a standard curve
The ratio C of the peak areas in the S2 series standard working solution is measured 1 /C 0 、C 2 /C 0 、C 3 /C 0 Carrying out linear regression analysis on the mass concentration of the peanut oil to obtain a standard curve linear regression equation;
s5, calculating the mass concentration of peanut oil in the sample to be detected
The ratio C of the peak areas in the sample solution of S1 will be measured 1 /C 0 、C 2 /C 0 、C 3 /C 0 Substituting the standard curve linear regression equation of S4, and calculating the mass concentration of peanut oil in the sample to be detected.
Further, the concentration of the internal standard in the sample solution of S1 was 5. Mu.g/kg; the concentration of the internal standard in the S2 series of standard working solutions was 5. Mu.g/kg.
Furthermore, the extraction head of the SPME method is a PDMS/DVB extraction head.
Further, in S3, the extraction procedure using PDMS/DVB extraction head is as follows:
the sample was equilibrated at 80 ℃ for 10min, then the PDMS/DVB extraction head was extended into the sample bottle and equilibrated at 80 ℃ for 30min in headspace, the sample bottle was placed on the shaker with the shaker on and off times of 10s and 5s, respectively.
Further, in S3, the GC/MS conditions are as follows:
the chromatographic column is TG-5MS;
the temperature-raising program is as follows: keeping the temperature at 40 ℃ for 5min, rising to 60 ℃ at 5 ℃/min, rising to 120 ℃ at 3 ℃/min, rising to 210 ℃ at 5 ℃/min, and keeping the temperature for 12min;
EI source, transmission line temperature 280 deg.C, ion source temperature 300 deg.C, scanning range 35-450m/z.
Furthermore, the peak time of the internal standard 2-methyl-3-heptanone is 13.35min; the peak time of the separated phenylacetaldehyde is 18.42min; the peak time of the separated 3-ethyl-2, 5-dimethyl pyrazine is 20.15min; the peak time of the isolate 4-vinyl-2-methoxyphenol was 30.96 minutes.
Further, in S2, the mass percentages of the series of standard working solutions are 1%, 2%, 5%, 10%, 20%, 50% and 100%, respectively.
The invention has the beneficial effects that:
1. the method provided by the invention has the advantages that the sampling amount is small, no complex sample pretreatment is needed, no chemical reagent is involved, three characteristic volatile components in peanut oil, namely phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol, are in direct proportion to the content of the peanut oil in other vegetable oils, and a method for detecting the incorporation of the peanut oil into the edible oil based on the volatile components is established based on the method.
2. According to the method, an internal standard method is adopted, 3 characteristic volatile components, namely phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol, in a sample are quantitatively detected through SPME-GC/MS, the ratio of the peak area of the 18.42min isolate phenylacetaldehyde, the 20.15min isolate 3-ethyl-2, 5-dimethyl pyrazine and the 30.96min isolate 4-vinyl-2-methoxyphenol to the internal standard peak area is calculated, and the content of peanut oil doped in the sample is calculated through a standard curve, so that quantitative detection of the peanut oil content in the sample is realized. The method has the advantages of good reliability, simplicity, convenience, rapidness and the like, and can relatively accurately analyze the relative content of peanut oil in edible vegetable oil and judge whether the edible vegetable oil is adulterated.
Drawings
Fig. 1 is a total ion flow diagram of the tea oil of 100% purity of example 1.
FIG. 2 is a total ion flow diagram of rapeseed oil of 100% purity in example 1.
FIG. 3 is a total ion flow chart of 100% purity rice oil in example 1.
Fig. 4 is a total ion flow diagram of 100% purity soybean oil in example 1.
Fig. 5 is a total ion flow diagram of 100% purity sunflower seed oil of example 1.
Fig. 6 is a total ion flow chart of sesame oil of 100% purity in example 1.
FIG. 7 is a GC-MS total ion flow diagram for example 2 with 100% peanut oil.
FIG. 8 is a GC-MS total ion flow diagram for example 2 with 10% peanut oil.
FIG. 9 is a GC-MS total ion flow diagram for example 2 with 1% peanut oil.
FIG. 10 is a mass spectrum of the separated peak material at 18.42min retention time.
FIG. 11 is a mass spectrum of the separated peak material at 20.15min retention time.
FIG. 12 is a mass spectrum of the separated peak material at 30.96min retention time.
FIG. 13 shows the ratio of peak areas C on the abscissa of peanut oil mass concentration in example 2 1 /C 0 、C 2 /C 0 、C 3 /C 0 A standard curve is plotted for the ordinate. (a) To be in peak area ratio C 1 /C 0 A standard curve is plotted for the ordinate. (b) To be in peak area ratio C 2 /C 0 A standard curve is plotted for the ordinate. (c) To be in peak area ratio C 3 /C 0 A standard curve is plotted for the ordinate.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The reagents, materials and experimental instruments related to the embodiment of the invention are as follows:
A. reagents and materials
Internal standard 2-methyl-3-heptanone (1 mg/L, aba Ding Shiji Co., ltd.);
the rest of the reagents and consumables, unless specified otherwise, are commercially available.
B. Experimental instrument
TSQ 8000Evo triple quadrupole gas chromatograph with automatic solid phase microextraction device (Thermo, siemens, U.S.A.);
column TG-5MS (30 m. Times.0.25 mm,0.25 μm, sieimer, USA).
The invention provides a quantitative detection method for rapeseed oil doped in edible vegetable oil, which comprises the following steps:
s1, pretreatment of a sample to be tested
Adding 2-methyl-3-heptanone serving as an internal standard into a sample to be detected to prepare a sample solution; wherein the concentration of the internal standard in the sample solution of S1 is 5. Mu.g/kg;
s2, standard working solution preparation
Peanut oil is added into base oil, and 2-methyl-3-heptanone is used as an internal standard to prepare a series of standard working solutions with the mass percent of 1% -100%; wherein the concentration of the internal standard in the series of standard working solutions of S2 is 5 mug/kg;
s3, SPME-GC/MS quantitative detection
The extraction head adopting SPME method is used for respectively adsorbing the sample solution of S1 and the serial standard working solution of S2, analyzing the extraction head adsorbing volatile components by GC/MS and quantifying the volatile components, and then calculating the peak area C of the phenylacetaldehyde separated in 18.42min 1 Peak area C of isolate 3-ethyl-2, 5-dimethylpyrazine at 20.15min 2 Peak area C of isolate 4-vinyl-2-methoxyphenol of 30.96min 3 And internal standard peak area C 0 Ratio C of (2) 1 /C 0 、C 2 /C 0 、C 3 /C 0 ；
The extraction head of the SPME method is a PDMS/DVB extraction head; the extraction procedure using PDMS/DVB extraction head was as follows:
the sample was equilibrated at 80 ℃ for 10min, then the PDMS/DVB extraction head was extended into the sample bottle and equilibrated at 80 ℃ for 30min in headspace, the sample bottle was placed on the shaker with the shaker on and off times of 10s and 5s, respectively.
The GC/MS conditions were as follows:
1) The chromatographic column is TG-5MS,30m x 0.25mm x 0.25 μm;
2) The temperature-raising program is as follows: keeping the temperature at 40 ℃ for 5min, rising to 60 ℃ at 5 ℃/min, rising to 120 ℃ at 3 ℃/min, rising to 210 ℃ at 5 ℃/min, and keeping the temperature for 12min;
3) The temperature of the sample inlet is 210 ℃;
4) The temperature of the transmission line is 280 ℃;
5) EI source, ion source temperature 300 ℃;
6) The carrier gas is helium;
7) The flow rate of the column is 1mL/min;
8) Split ratio: sample introduction without diversion;
9) Mass scan range: scanning range is 35-450m/z;
10 Scanning mode): full SCAN.
The peak time of the internal standard 2-methyl-3-heptanone is 13.35min; the peak time of the separated phenylacetaldehyde is 18.42min; the peak time of the separated 3-ethyl-2, 5-dimethyl pyrazine is 20.15min; the peak time of the isolate 4-vinyl-2-methoxyphenol was 30.96 minutes.
S4, drawing a standard curve
The ratio C of the peak areas in the S2 series standard working solution is measured 1 /C 0 、C 2 /C 0 、C 3 /C 0 Performing linear regression analysis on the mass concentration of the rapeseed oil to obtain a standard curve linear regression equation;
s5, calculating the mass concentration of the rapeseed oil in the sample to be detected
The ratio C of the peak areas in the sample solution of S1 will be measured 1 /C 0 、C 2 /C 0 、C 3 /C 0 Substituting the standard curve linear regression equation of S4, and calculating the mass concentration of peanut oil in the sample to be detected.
The adulteration judgment is as follows: if the total ion flow graph of the sample shows no separation peaks at 18.42min (phenylacetaldehyde), 20.15min (3-ethyl-2, 5-dimethylpyrazine) and 30.96min (4-vinyl-2-methoxyphenol), no mass spectrum as shown in FIG. 10 is detected, i.e. it is determined that no peanut oil is incorporated in the sample or that the peanut oil is incorporated in the sample in an amount of less than 6%. If separated peaks exist at 18.42min, 20.15min and 30.96min in the total ion flow graph of the sample, and a mass spectrum shown in figure 10 is detected, calculating the ratio of the peak area to the internal standard peak area under the three peak-out times, and calculating through a standard curve to obtain the peanut oil content.
The following quantitative determination of the adulteration amount of peanut oil is carried out by taking tea oil as base oil, and the specific operation is as follows.
Example 1
Determination of volatile components of different pure vegetable oils:
(1) Two different sources of 7 pure vegetable oils were collected: tea oil, peanut oil, rice oil, soybean oil, sunflower seed oil, sesame oil and rapeseed oil;
(2) Accurately weighing 4.00g of pure vegetable oil sample into a 20mL brown flat bottom headspace solid-phase microextraction bottle, then adding 20 mu L of 2-methyl-3-heptanone with the concentration of 1mg/L as an internal standard, and enabling the concentration of the internal standard sample solution to be 5 mu g/kg; wherein, the 20mL brown flat bottom headspace solid phase microextraction bottle needs to be cleaned before use and is placed in a 250 ℃ oven for drying for 12 hours for standby.
(3) The sample volatile component analysis was performed using a TSQ 8000Evo triple quadrupole gas chromatograph (Thermo) with an automated solid phase microextraction device.
The extraction procedure is as follows: the sample is balanced for 10min at 80 ℃, the PDMS/DVB extraction head is extended into a sample bottle, the suction and the balance are carried out for 30min at 80 ℃, the sample bottle is placed on an oscillator, and the opening time and the closing time of the oscillator are respectively 10s and 5s.
The GC/MS conditions were: the chromatographic column is TG-5MS; the temperature-raising program is as follows: keeping the temperature at 40 ℃ for 5min, rising to 60 ℃ at 5 ℃/min, rising to 120 ℃ at 3 ℃/min, rising to 210 ℃ at 5 ℃/min, and keeping the temperature for 12min; EI source, transmission line temperature 280 ℃, ion source temperature 300 ℃, scanning m/z range 35-450.
The total ion flow diagram of the pure vegetable oil (tea oil, rice oil, soybean oil, sunflower seed oil, sesame oil and rapeseed oil) is shown in figures 1-6. The total ion flow diagram of 100% purity peanut oil is shown in figure 7. From fig. 1-7, almost all of the total ion flow diagrams of the vegetable oils showed no peaks at 18.42min, 20.15min and 30.96min, while the peanut oil showed distinct separation peaks at 18.42min, 20.15min and 30.96min, and only rapeseed oil showed separation peaks at 20.15min, with peak areas much lower than that of pure peanut oil.
Example 2
The tea oil is taken as base oil, peanut oil with the mass percent of 1%, 2%, 5%, 10%, 20%, 50% and 100% is added, and a standard curve is drawn. The specific operation is as follows:
(1) 8 clean beakers are prepared and numbered;
(2) 100g, 99g, 98g, 95g, 90g, 80g, 50g and 0g of tea oil are respectively added into corresponding beakers, then 0g, 1g, 2g, 5g, 10g, 20g, 50g and 100g of peanut oil are added, and a magnetic stirrer is used for evenly stirring at room temperature, so as to obtain 8 parts of mixed oil samples;
(3) Accurately weighing 4.00g of mixed oil sample respectively, and detecting and analyzing volatile components according to the method of example 1; peak areas C occurring at 18.42min, 20.15min and 30.96min were recorded 1 、C 2 、C 3 And inner partPeak area C 0 And calculate the ratio C of peak areas 1 /C 0 、C 2 /C 0 And C 3 /C 0 ；
(4) The peanut oil mass concentration is taken as an abscissa, and the peak area ratio C 1 /C 0 、C 2 /C 0 And C 3 /C 0 The standard curve is plotted on the ordinate as shown in fig. 13.
The GC-MS total ion flow diagrams containing 100%, 10%, 1% peanut oil are shown in FIGS. 7-9. Mass spectra of the separated peak substances at 18.42min, 20.15min, 30.96min retention time are shown in fig. 10-12. The peanut oil mass concentration is taken as an abscissa, and the peak area ratio C 1 /C 0 、C 2 /C 0 And C 3 /C 0 The standard curve plotted for the ordinate is shown in fig. 13. As shown in the figure, C 1 /C 0 、C 2 /C 0 And C 3 /C 0 In a proportional relationship (5% -50%) with the mass concentration of peanut oil, the linear equations are respectively: y=0.360X-0.024 (R 2 ＝0.9882)、Y＝0.275X-0.013(R 2 ＝0.9992)、Y＝1.7305X-0.087(R 2 ＝0.9924)。
Example 3
The mass concentration of peanut oil in the oil sample to be measured is calculated by taking tea oil as base oil and independently doping 6%, 7%, 8% and 12% of peanut oil. The specific operation is as follows:
(1) Preparing 4 clean beakers and numbering;
(2) 94g, 93g, 96g and 88g of tea oil are respectively added into corresponding beakers, and then 6g, 7g, 8g and 12g of peanut oil are respectively added; the magnetic stirrer is uniform at room temperature, and thus, the peanut oil-tea oil mixed oil with the concentration of 6%, 7%, 8% and 12% is obtained;
(3) Accurately weighing 4.00g of mixed oil samples respectively, and detecting and analyzing volatile components according to the method of the example 1; peak areas C occurring at 18.42min, 20.15min and 30.96min were recorded 1 、C 2 、C 3 And internal standard peak area C 0 And calculate the ratio C of peak areas 1 /C 0 、C 2 /C 0 And C 3 /C 0 ；
(4) The calculated peak area ratio C 1 /C 0 、C 2 /C 0 And C 3 /C 0 Substituting the standard curve linear regression equation of example 2, and calculating the mass concentration of peanut oil in the mixed oil sample to be measured, and the result is shown in table 1.
TABLE 1 detection results of peanut oil incorporation into tea oil
A * B, C are respectively expressed according to C 1 /C 0 、C 2 /C 0 And C 3 /C 0 Adulteration (%) calculated from peanut oil concentration standard curve;
average recovery/% = (calculated average ratio of peanut oil/actual ratio of peanut oil) x 100%;
the symbol "indicates that the corresponding peak was not present, and the content could not be calculated.
According to the standard curve, when about 5% of peanut oil is added in the peanut oil-tea oil mixture, the separation peaks of three characteristic volatile components start to appear. Thus, the peanut oil-tea oil blends at 6%, 7%, 8% and 12% add-ons were tested to determine the lowest concentration of peanut oil in the oil samples to be tested. In example 3, the volatile component was analyzed by the method of example 1, and the peak area ratio C was calculated 1 /C 0 、C 2 /C 0 And C 3 /C 0 The measured blending ratio was calculated using the standard curve of example 2, and the results are shown in table 1. As can be seen from Table 1, by the method of the present invention, when the tea oil is blended with more than 7% peanut oil, it is possible to accurately determine whether the peanut oil is present in the sample. Meanwhile, when the mass ratio of the doped peanut oil is 7%, 8% and 12%, the measurement results of the method are respectively4.38% -4.42%, 5.67% -7.54% and 13.57% -16.65%, the recovery rate is between 66.33% -127.14%, and the variation coefficient is lower than 9.54%.
Example 4
The tea oil is taken as base oil, 2% of different peanut oil, rice oil, soybean oil, sunflower seed oil and sesame oil are respectively mixed, and then 8% of peanut oil is added, so that the mass concentration of the peanut oil in an oil sample to be detected is calculated. The specific operation is as follows:
(1) Preparing 5 clean beakers and numbering;
(2) Adding 90g of tea oil into a corresponding beaker respectively, and then adding 2g of peanut oil, rice oil, soybean oil, sunflower seed oil and sesame oil respectively, and adding 8g of peanut oil respectively; the magnetic stirrer was uniform at room temperature to obtain 5 parts of a mixed oil sample.
(3) Accurately weighing 4.00g of mixed oil samples respectively, and detecting and analyzing volatile components according to the method of the example 1; peak areas C occurring at 18.42min, 20.15min and 30.96min were recorded 1 、C 2 、C 3 And internal standard peak area C 0 And calculate the ratio C of peak areas 1 /C 0 、C 2 /C 0 And C 3 /C 0 ；
(4) The calculated peak area ratio C 1 /C 0 、C 2 /C 0 And C 3 /C 0 Substituting the standard curve linear regression equation of example 2, and calculating the mass concentration of peanut oil in the mixed oil sample to be measured, and the result is shown in table 2.
Table 2 detection results of blending rapeseed oil and different vegetable oils into tea oil
A * B, C are respectively expressed according to C 1 /C 0 、C 2 /C 0 And C 3 /C 0 Adulteration (%) calculated from peanut oil concentration standard curve;
average recovery/% = (calculated average ratio of peanut oil/actual ratio of peanut oil) x 100%;
&the data preceding the symbol "/" are expressed in terms of C 1 /C 0 、C 2 /C 0 And C 3 /C 0 The adulteration amount, the recovery rate and the variation coefficient are calculated by the average value of the three; data following the symbol "/" indicates removal of C 2 /C 0 And the calculated adulteration amount, recovery rate and variation coefficient.
In example 4, the volatile component was analyzed by the method in example 1, and the peak area ratio C was calculated 1 /C 0 、C 2 /C 0 And C 3 /C 0 The measured blending ratio was calculated using the standard curve of example 2, and the results are shown in table 2. As can be seen from Table 2, by the method of the present invention, the presence or absence of peanut oil in a sample can be accurately determined. Meanwhile, when the mass ratio of the mixed peanut oil is 8%, the mixing fake can be accurately judged, the measured result is between 6.68% and 9.82%, the recovery rate is between 83.50% and 100.25%, and the variation coefficient is lower than 21.83%. The accuracy is better.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (3)
1. A method for detecting the incorporation of peanut oil into edible oil based on volatile components is characterized in that 2-methyl-3-heptanone is used as an internal standard, the characteristic volatile components of phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol in a sample are quantitatively detected through SPME-GC/MS, the ratio of peak area corresponding to the separated components of phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol to the internal standard peak area is calculated, and the content of the incorporated peanut oil in the sample is calculated through a standard curve, so that the quantitative detection of the peanut oil content in the sample is realized; wherein, the characteristic volatile components of phenylacetaldehyde, 3-ethyl-2, 5-dimethyl pyrazine and 4-vinyl-2-methoxyphenol in the peanut oil are in direct proportion to the content of the peanut oil in other edible oils; the other edible oil is at least one of tea oil, rapeseed oil, rice oil, soybean oil, sunflower seed oil and sesame oil;
the specific method comprises the following steps:
s1, preparing a sample solution
Adding 2-methyl-3-heptanone serving as an internal standard into a sample to be detected to prepare a sample solution;
s2, standard working solution preparation
Peanut oil is added into base oil, and 2-methyl-3-heptanone is used as an internal standard to prepare a series of standard working solutions with the mass percent of 1% -100%;
s3, SPME-GC/MS quantitative detection
The extraction head adopting SPME method is used for respectively adsorbing the sample solution of S1 and the serial standard working solution of S2, analyzing the extraction head adsorbing volatile components by GC/MS and quantifying the volatile components, and then calculating the peak area C of the separated phenylacetaldehyde 1 Peak area C of isolate 3-ethyl-2, 5-dimethylpyrazine 2 Peak area C of isolate 4-vinyl-2-methoxyphenol 3 And internal standard peak area C 0 Ratio C of (2) 1 /C 0 、C 2 /C 0 、C 3 /C 0 ；
S4, drawing a standard curve
The ratio C of the peak areas in the S2 series standard working solution is measured 1 /C 0 、C 2 /C 0 、C 3 /C 0 Carrying out linear regression analysis on the mass concentration of the peanut oil to obtain a standard curve linear regression equation;
s5, calculating the mass concentration of peanut oil in the sample to be detected
The ratio C of the peak areas in the sample solution of S1 will be measured 1 /C 0 、C 2 /C 0 、C 3 /C 0 Substituting the standard curve linear regression equation of S4, and calculating the mass concentration of peanut oil in the sample to be detected;
s3, the extraction head of the SPME method is a PDMS/DVB extraction head;
the extraction procedure using PDMS/DVB extraction head was as follows:
balancing the sample at 80 ℃ for 10min, then extending the PDMS/DVB extraction head into a sample bottle, balancing the suction of the sample bottle at 80 ℃ for 30min, placing the sample bottle on an oscillator, wherein the opening and closing time of the oscillator is respectively 10s and 5s;
the GC/MS conditions were as follows:
the chromatographic column is TG-5MS;
the temperature-raising program is as follows: keeping the temperature at 40 ℃ for 5min, rising to 60 ℃ at 5 ℃/min, rising to 120 ℃ at 3 ℃/min, rising to 210 ℃ at 5 ℃/min, and keeping the temperature for 12min;
EI source, transmission line temperature 280 deg.C, ion source temperature 300 deg.C, scanning range 35-450m/z.
2. The method for volatile component-based detection of peanut oil incorporation in an edible oil according to claim 1, wherein the concentration of the internal standard in the sample solution of S1 is 5 μg/kg; the concentration of the internal standard in the S2 series of standard working solutions was 5. Mu.g/kg.
3. The method for detecting the incorporation of peanut oil in an edible oil based on volatile components according to claim 1, wherein in S2 the mass percentage of peanut oil in the series of standard working solutions is 1%, 2%, 5%, 10%, 20%, 50% and 100%, respectively.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014002082A (en) * | 2012-06-20 | 2014-01-09 | Chikuno Shokuhin Kogyo Kk | Quantitative method of volatile organic compound |
| WO2017173638A1 (en) * | 2016-04-07 | 2017-10-12 | 浙江大学 | Method for using squalene as identification marker of olive oil and camellia seed oil |
-
2021
- 2021-11-03 CN CN202111294833.XA patent/CN114019050B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014002082A (en) * | 2012-06-20 | 2014-01-09 | Chikuno Shokuhin Kogyo Kk | Quantitative method of volatile organic compound |
| WO2017173638A1 (en) * | 2016-04-07 | 2017-10-12 | 浙江大学 | Method for using squalene as identification marker of olive oil and camellia seed oil |
Non-Patent Citations (10)
| Title |
|---|
| 3种坚果油的挥发性成分提取及关键风味成分分析;贾潇 等;中国油脂;第45卷(第7期);第35-41页 * |
| Kai-Min Yang 等.Headspace Solid-Phase Microextraction Analysis of Volatile Components in Peanut Oil.Molecules.2021,第26卷(第11期),第1-16页. * |
| QuEChERS气相色谱质谱法测定花生油中17种邻苯二甲酸酯类物质;高霞 等;粮油食品科技;20200921;第28卷(第05期);第138-143页 * |
| 刘云花 等.花生饼粕及花生壳烘烤风味分析.食品科学.2017,第38卷(第02期),第146-153页. * |
| 刘晓君 等.花生油挥发性风味成分的鉴定.中国油脂.2008,(第08期),第40-42页. * |
| 史文青.花生及花生油挥发性气味真实性成分的鉴定.中国优秀硕士学位论文全文数据库 工程科技I辑 2015年 .2013,(第05期),第49-55页. * |
| 张文刚 等.不同品种青稞炒制后挥发性风味物质GC-MS分析.食品科学.2019,第40卷(第08期),第192-201页. * |
| 王李平 等.花生油挥发性风味物质SPME-GC/MS指纹图谱的研究.食品工业.2020,第41卷(第07期),第162-165页. * |
| 花生及花生油挥发性气味真实性成分的鉴定;史文青;中国优秀硕士学位论文全文数据库 工程科技I辑(第05期);第49-61页 * |
| 花生油香气特征在其属性识别中的初步应用;李苑雯 等;花生油香气特征在其属性识别中的初步应用;第39卷(第7期);第193-199页 * |
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