CN106526031A - Method for distinguishing adulterated peanut oil - Google Patents
Method for distinguishing adulterated peanut oil Download PDFInfo
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- CN106526031A CN106526031A CN201611205374.2A CN201611205374A CN106526031A CN 106526031 A CN106526031 A CN 106526031A CN 201611205374 A CN201611205374 A CN 201611205374A CN 106526031 A CN106526031 A CN 106526031A
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- CN
- China
- Prior art keywords
- arachidis hypogaeae
- peanut oil
- oleum arachidis
- hypogaeae semen
- extraction
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- 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.)
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Classifications
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention relates to a method for distinguishing adulterated peanut oil. The method includes the following steps: conducting pretreatment, wherein a peanut oil sample is subjected to pretreatment; conducting headspace microextraction, wherein an extraction head is activated so as to remove impurities on the surface of the extraction head, and a headspace solid phase microextraction technology is used for conducting aromatic substance extraction on the pretreated peanut oil sample; conducting analysis, wherein extracted aromatic substances are analyzed by a gas chromatograph-mass spectrometer; processing experimental maps with a Xcalibur software to obtain related data, and conducting qualitative analysis on peanut essences by using ethyl maltol and glyceryl triacetate as characteristic substances. The combination of the headspace solid phase microextraction and the gas chromatograph-mass spectrometer is used for separating and identifying volatile substances of the peanut oil and the peanut essences; based on the analysis on inherent endogenous substances in the peanut oil and the characteristic aromatic substances of the peanut essences, peanut oil adulteration distinguishing is conducted, and the method is of great significance to protect the lawful rights of peanut oil producers and consumers.
Description
Technical field
The present invention relates to a kind of detection method, more particularly to a kind of discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen, belong to food analyses
Detection field.
Background technology
Heavy fragrant peanut oil has unique local flavor, and containing adjoint beneficial to human body such as abundant Vitamin E, sterol
Material, it is deep to be liked by consumer.Heavy fragrant peanut oil has become higher, the expensive product of nutritive value in edible vegetable oil
Product.
China is the big edible vegetable oil country of consumption of the first in the world, and the great insufficiency of supply-demand in market and heavy fragrant peanut oil are unique
Local flavor and higher price positioning so that it is serious that pseudo- phenomenon is mixed in market.National standard《Oleum Arachidis hypogaeae semen》Middle regulation " must not in Oleum Arachidis hypogaeae semen
Mixed with other edible oil and unedible oil, any essence and spice must not be added ".However, some illegal retailers are to obtain in recent years
Sudden huge profits are taken, it is adulterated in Oleum Arachidis hypogaeae semen repeatedly, low value oil is blent using essence and flavoring agent and pretend to be heavy fragrant peanut oil, adulterate.It is dense
The illegal addition of the adulterated and banned substance of fragrant flower oil generation constitutes a serious threat to the health of the people.Long-term consumption not only can
Harm is brought to health, has also upset the order of domestic edible oil market.In order to protect, producers and consumers' is legal
Rights and interests, strengthen the production and selling supervision of heavy fragrant peanut oil, set up a set of science, simplicity, quick, accurate and effective mix pseudo- flower
The discrimination method of oil generation is particularly important.
Oleum Arachidis hypogaeae semen adulteration detection method mainly has spectrographic method, nuclear magnetic resonance method, isotope method, gas chromatography etc. at present.
Wherein spectrographic method needs a large amount of sample modelings, and testing cost is high；Gas chromatography mainly by detect fatty acid species and content come
Whether discriminating mixes puppet, and accuracy is low；Isotope method and nuclear magnetic resonance method apparatus expensive and detection method is still immature, it is difficult to extensively
Popularization and application.
The content of the invention
A kind of deficiency that the present invention is present for existing Oleum Arachidis hypogaeae semen adulteration detection method, there is provided discriminating side for mixing pseudo- Oleum Arachidis hypogaeae semen
Method.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen, comprises the steps：
1) pretreatment：Semen arachidis hypogaeae oil samples are carried out into pretreatment；
2) head space micro-extraction：Activation extracting head, to remove the impurity of extraction head surface, using headspace solid-phase microextraction technology
To step 1) in pretreated Semen arachidis hypogaeae oil samples carry out the extraction of aroma substance；
3) analyze：The aroma substance for extracting is analyzed using gas chromatograph-mass spectrometer；
4) by obtaining related data using Xcalibur software processes experimental patterns, using ethylmaltol and triacetic acid
Glyceride carries out qualitative analyses as characteristic material to peanut essence.
Further, the capillary column that gas chromatogram is used in the gas chromatograph-mass spectrometer be DB-5MS chromatographic columns, column oven liter
Warm program is 40 DEG C of holding 2min, is warming up to 220 DEG C with the heating rate of 5 DEG C/min, keeps 10min, temperature of vaporization chamber：250
DEG C, helium flow velocity 0.8mL/min, input mode is Splitless injecting samples.
Further, in the gas chromatograph-mass spectrometer Mass Spectrometry Conditions be electron impact ion source energy 70eV, ion source temperature 200
DEG C, 200 μ A of filament emission current, 250 DEG C of interface temperature, full spectrum scanning, quality of scanning scope m/z 32-402.
Further, step 2) in extraction temperature be 45-50 DEG C, extraction time is 40-50min.
Further, step 1) described in the method for pretreatment be that Oleum Arachidis hypogaeae semen is placed in ml headspace bottle in 45-50 DEG C of thermostatted water
Heating balance 20-30min in bath.
Further, step 2) described in extracting head be solid-phase microextraction hand sampling (DVB/CAR/PDMS) extracting head,
50/30μm DVB/CAR on PDMS。
Further, step 2) described in activate extracting head method be that the injector temperature of gas chromatograph-mass spectrometer is set to
270 DEG C, then extracting head insertion gas chromatograph-mass spectrometer injection port is activated, soak time is 30-60min.
The present invention is computed machine examination rope and NIST by obtaining related data using Xcalibur software processes experimental patterns
Spectrum storehouse (data of 107000 compounds) and Wiley spectrums storehouse (data of 320000 compounds) matchings determine unknown compound
Title and relevant information, only report RSI (matching degree) more than 800 (maximum is 1000) related qualification result.Each component
Relative amount be calculated by areas of peak normalization method.
The invention has the beneficial effects as follows：
1) present invention combines gas chromatography mass spectrometry, the volatilization of isolation identification Oleum Arachidis hypogaeae semen and peanut essence using headspace solid-phase microextraction
Property material, by analyze Oleum Arachidis hypogaeae semen in intrinsic endogenous thing and peanut essence feature aroma substance, carry out Oleum Arachidis hypogaeae semen and mix puppet
Differentiate, to protecting Oleum Arachidis hypogaeae semen producers and consumers' legitimate rights and interests significant.
2) test limit is low, and up to 0.1%, accuracy is high, and testing cost is low, easy to operate.
Specific embodiment
The principle and feature of the present invention are described below in conjunction with example, example is served only for explaining the present invention, and
It is non-for limiting the scope of the present invention.
Embodiment 1：
The determination method of characteristic material is as follows：
1) sample collection：Take the heavy fragrant peanut oil 2 of different brands, different manufacturers peanut essence 2；
2) 2g heavy fragrant peanut oils are taken or essence is placed in 15mL ml headspace bottles, after adding stirrer, ml headspace bottle is placed in into 50 DEG C
In water bath with thermostatic control, heating balance 20min, inserts activated good SPME extracting heads by dottle pin with holes, after releasing extracting head,
Under conditions of 50 DEG C of waters bath with thermostatic control after headspace absorption 40min, 5min is parsed in 250 DEG C.
3) analytical conditions for gas chromatography：Capillary column：DB-5MS chromatographic columns (30mm × 0.25mm × 0.25 μm)；Gas phase post
Warm heating schedule：40 DEG C of holding 2min, are warming up to 220 DEG C with the heating rate of 5 DEG C/min, keep 10min；Temperature of vaporization chamber：
250℃；Helium flow velocity 0.8mL/min；Input mode：Splitless injecting samples；
4) Mass Spectrometry Conditions：Electron impact ion source (EI)；Electron energy 70eV；200 DEG C of ion source temperature；Filament transmitting electricity
Flow 200 μ A；Interface temperature is 250 DEG C；Full spectrum scanning, quality of scanning scope m/z32-402；
5) related data is obtained by Xcalibur software processes experimental patterns, be computed machine examination rope and compose storehouse with NIST
(data of 107000 compounds) and Wiley spectrum storehouse (data of 320000 compounds) matching determines the name of unknown compound
Claim and relevant information, only report related qualification results of the RSI (matching degree) more than 800 (maximum is 1000).The phase of each component
Content is calculated by areas of peak normalization method.Table 1 is peanut oil essence and heavy fragrant peanut oil key aroma material GC-MS
Analysis result.
1 peanut essence of table and heavy fragrant peanut oil key aroma material GC-MS analysis results
Numerical value in table 1 shows that the species of the aroma substance in peanut essence and heavy fragrant peanut oil is existed significantly
Difference, containing abundant Pyrazine material in heavy fragrant peanut oil, and pyrazine species is more single in essence；Contain in peanut oil essence
Substantial amounts of ethylmaltol and glyceryl triacetate, and do not detect in heavy fragrant peanut oil, therefore, we using ethylmaltol and
Glyceryl triacetate as peanut essence characteristic material be used for Oleum Arachidis hypogaeae semen in peanut essence qualitative detection.
Embodiment 2：
In Oleum Arachidis hypogaeae semen, the test limit of peanut essence determines that method is as follows：
1) sample preparation：The Semen arachidis hypogaeae for adding 0.1%, 0.2%, 0.5% (mass fraction) successively in Semen arachidis hypogaeae mixed oil is fragrant
Essence, preparation mix pseudo- Oleum Arachidis hypogaeae semen；
2) what is prepared in taking 2g steps 1 respectively mixes pseudo- Oleum Arachidis hypogaeae semen, is placed in ml headspace bottle, after adding stirrer, by ml headspace bottle
Heating balance 20min in 50 DEG C of waters bath with thermostatic control is placed in, activated good SPME extracting heads are inserted by dottle pin with holes, extraction is released
After taking head, under conditions of 50 DEG C of waters bath with thermostatic control after headspace absorption 40min, 5min is parsed in 250 DEG C；
3) GC conditions：Capillary column：DB-5MS chromatographic columns (30mm × 0.25mm × 0.25 μm)；Gas phase column temperature liter
Warm program：40 DEG C of holding 2min, are warming up to 220 DEG C with the heating rate of 5 DEG C/min, keep 10min；Temperature of vaporization chamber：250
℃；Helium flow velocity 0.8mL/min；Input mode：Splitless injecting samples；
4) Mass Spectrometry Conditions：Electron impact ion source (EI)；Electron energy 70eV；200 DEG C of ion source temperature；Filament transmitting electricity
Flow 200 μ A；Interface temperature is 250 DEG C；Full spectrum scanning, quality of scanning scope m/z32-402；
5) related data is obtained by Xcalibur software processes experimental patterns, be computed machine examination rope and compose storehouse with NIST
(data of 107000 compounds) and Wiley spectrum storehouse (data of 320000 compounds) matching determines the name of unknown compound
Claim and relevant information, only report related qualification results of the RSI (matching degree) more than 800 (maximum is 1000).The phase of each component
Content is calculated by areas of peak normalization method.Table 2 differentiates the GC-MS analysis knots of material for mixing characteristic in pseudo- Oleum Arachidis hypogaeae semen
Really.The mixed oil for adding 0.1% peanut essence can be discerned the false from the genuine completely.
Table 2 adds the analysis result for mixing pseudo- Oleum Arachidis hypogaeae semen property material of peanut essence
Embodiment 3：
A kind of discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen, comprises the steps：
1) sample pretreatment：Semen arachidis hypogaeae oil samples to be detected are placed in 15mL ml headspace bottles, after adding stirrer, by head space
Bottle is placed in heating balance 20min in 50 DEG C of waters bath with thermostatic control；
2) extracting head is activated, using solid-phase microextraction hand sampling (DVB/CAR/PDMS) extracting head, 50/30 μm of DVB/
CAR on PDMS, extracting head insertion gas chromatograph-mass spectrometer injection port is activated, and injector temperature is set to 270 DEG C, during activation
Between be 30-60min；
3) activated good SPME extracting heads are inserted in ml headspace bottle by dottle pin with holes, after releasing extracting head, 50
Under conditions of DEG C water bath with thermostatic control after headspace absorption 40min, 5min are parsed in 250 DEG C；
4) aroma substance drawn in extracting head is carried out into gaschromatographic mass spectrometric analysises, GC conditions after：Capillary
Tubing string：DB-5MS chromatographic columns (30mm × 0.25mm × 0.25 μm)；Gas phase column temperature heating schedule：40 DEG C holding 2min, with 5 DEG C/
The heating rate of min is warming up to 220 DEG C, keeps 10min；Temperature of vaporization chamber：250℃；Helium flow velocity 0.8mL/min；Enter sample prescription
Formula：Splitless injecting samples；
Mass Spectrometry Conditions：Electron impact ion source (EI)；Electron energy 70eV；200 DEG C of ion source temperature；Filament emission current
200μA；Interface temperature is 250 DEG C；Full spectrum scanning, quality of scanning scope m/z32-402；
5) related data is obtained by Xcalibur software processes experimental patterns, be computed machine examination rope and compose storehouse with NIST
(data of 107000 compounds) and Wiley spectrum storehouse (data of 320000 compounds) matching determines the name of unknown compound
Claim and relevant information, only report related qualification results of the RSI (matching degree) more than 800 (maximum is 1000).The phase of each component
Content is calculated by areas of peak normalization method.
6) qualitative analyses：If occurring in that the characteristic peak of ethylmaltol and glyceryl triacetate in testing result, prove
Really peanut essence is doped with Oleum Arachidis hypogaeae semen, if not occurring the feature of ethylmaltol and glyceryl triacetate in testing result
Peak, then prove undoped p peanut essence in Oleum Arachidis hypogaeae semen.
The foregoing is only presently preferred embodiments of the present invention, not to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (8)
1. a kind of discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen, it is characterised in that comprise the steps：
1) pretreatment：Semen arachidis hypogaeae oil samples are carried out into pretreatment；
2) head space micro-extraction：Activation extracting head, to remove the impurity of extraction head surface, using headspace solid-phase microextraction technology to step
It is rapid 1) in pretreated Semen arachidis hypogaeae oil samples carry out the extraction of aroma substance；
3) analyze：The aroma substance for extracting is analyzed using gas chromatograph-mass spectrometer；
4) it is by obtaining related data using Xcal ibur software processes experimental patterns, sweet using ethylmaltol and triacetic acid
Grease carries out qualitative analyses as characteristic material to peanut essence.
2. the discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen according to claim 1, it is characterised in that gas phase in the gas chromatograph-mass spectrometer
The capillary column that chromatograph is used is DB-5MS chromatographic columns, and column oven heating schedule is 40 DEG C of holding 2min, with the intensification of 5 DEG C/min
Ramp keeps 10min, temperature of vaporization chamber to 220 DEG C：250 DEG C, helium flow velocity 0.8mL/min, input mode are not shunt
Sample introduction.
3. the discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen according to claim 1, it is characterised in that mass spectrum in the gas chromatograph-mass spectrometer
Condition be electron impact ion source energy 70eV, 200 DEG C of ion source temperature, 200 μ A of filament emission current, 250 DEG C of interface temperature,
Full spectrum scanning, quality of scanning scope m/z 32-402.
4. the discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen according to claim 1, it is characterised in that step 2) in the temperature of extraction be
45-50 DEG C, extraction time is 40-50min.
5. the discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen according to claim 1, it is characterised in that step 1) described in pretreatment
Method is that Oleum Arachidis hypogaeae semen is placed in ml headspace bottle the heating balance 20-30min in 45-50 DEG C of water bath with thermostatic control.
6. the discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen according to claim 1, it is characterised in that step 2) described in extracting head
For solid-phase microextraction hand sampling (DVB/CAR/PDMS) extracting head, 50/30 μm of DVB/CAR on PDMS.
7. the discrimination method for mixing pseudo- Oleum Arachidis hypogaeae semen according to claim 1, it is characterised in that step 2) described in activation extraction
The method of head is that the injector temperature of gas chromatograph-mass spectrometer is set to 270 DEG C, then extracting head is inserted gas chromatograph-mass spectrometer injection port
Activated, soak time is 30-60min.
8. the discrimination method any one of a kind of claim 1-7 mixes the application in pseudo- discriminating field in Oleum Arachidis hypogaeae semen.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950321A (en) * | 2017-05-10 | 2017-07-14 | 中粮福临门食品营销有限公司 | A kind of peanut oil flavor substance content judges the method that peanut fries the seed time |
| CN107085048A (en) * | 2017-04-07 | 2017-08-22 | 青岛市食品药品检验研究院 | The detection method of content of olive oil in a kind of olive blending oil |
| CN109541050A (en) * | 2018-11-09 | 2019-03-29 | 重庆市食品药品检验检测研究院 | A kind of gas chromatography measures malt phenols content method in edible vegetable oil simultaneously |
| CN112067714A (en) * | 2020-08-26 | 2020-12-11 | 青岛市食品药品检验研究院（青岛市药品不良反应监测中心、青岛市实验动物和动物实验中心） | Method for determining peanut oil essence in peanut oil |
| CN112326811A (en) * | 2020-09-28 | 2021-02-05 | 中国石油化工股份有限公司 | Method for predicting content of single crude oil in mixed crude oil |
| CN112578060A (en) * | 2020-11-25 | 2021-03-30 | 青海大学 | Method for measuring volatile components of linseed oil and application thereof |
| CN114660189A (en) * | 2020-12-24 | 2022-06-24 | 益海嘉里金龙鱼粮油食品股份有限公司 | Method for detecting ethyl maltol in edible oil |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085048A (en) * | 2017-04-07 | 2017-08-22 | 青岛市食品药品检验研究院 | The detection method of content of olive oil in a kind of olive blending oil |
| CN106950321A (en) * | 2017-05-10 | 2017-07-14 | 中粮福临门食品营销有限公司 | A kind of peanut oil flavor substance content judges the method that peanut fries the seed time |
| CN109541050A (en) * | 2018-11-09 | 2019-03-29 | 重庆市食品药品检验检测研究院 | A kind of gas chromatography measures malt phenols content method in edible vegetable oil simultaneously |
| CN109541050B (en) * | 2018-11-09 | 2022-03-25 | 重庆市食品药品检验检测研究院 | Method for simultaneously determining content of maltol in edible vegetable oil by gas chromatography |
| CN112067714A (en) * | 2020-08-26 | 2020-12-11 | 青岛市食品药品检验研究院（青岛市药品不良反应监测中心、青岛市实验动物和动物实验中心） | Method for determining peanut oil essence in peanut oil |
| CN112326811A (en) * | 2020-09-28 | 2021-02-05 | 中国石油化工股份有限公司 | Method for predicting content of single crude oil in mixed crude oil |
| CN112578060A (en) * | 2020-11-25 | 2021-03-30 | 青海大学 | Method for measuring volatile components of linseed oil and application thereof |
| CN114660189A (en) * | 2020-12-24 | 2022-06-24 | 益海嘉里金龙鱼粮油食品股份有限公司 | Method for detecting ethyl maltol in edible oil |
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