CN108572225A - A kind of method that FaPEx-GC-MS/MS detects multi-tesidual pesticides in healthy food material simultaneously - Google Patents
A kind of method that FaPEx-GC-MS/MS detects multi-tesidual pesticides in healthy food material simultaneously Download PDFInfo
- Publication number
- CN108572225A CN108572225A CN201810378346.3A CN201810378346A CN108572225A CN 108572225 A CN108572225 A CN 108572225A CN 201810378346 A CN201810378346 A CN 201810378346A CN 108572225 A CN108572225 A CN 108572225A
- Authority
- CN
- China
- Prior art keywords
- fapex
- pesticides
- food material
- healthy food
- tesidual
- 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
- 239000000575 pesticide Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 36
- 235000001497 healthy food Nutrition 0.000 title claims abstract description 27
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract description 24
- 239000011159 matrix material Substances 0.000 claims abstract description 43
- 238000001514 detection method Methods 0.000 claims abstract description 32
- 230000014759 maintenance of location Effects 0.000 claims abstract description 24
- 239000012086 standard solution Substances 0.000 claims abstract description 19
- 238000000746 purification Methods 0.000 claims abstract description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 36
- 150000001875 compounds Chemical class 0.000 claims description 34
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 21
- 239000003905 agrochemical Substances 0.000 claims description 18
- 238000001819 mass spectrum Methods 0.000 claims description 18
- 238000002552 multiple reaction monitoring Methods 0.000 claims description 10
- 239000012159 carrier gas Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- RQBBFKINEJYDOB-UHFFFAOYSA-N acetic acid;acetonitrile Chemical compound CC#N.CC(O)=O RQBBFKINEJYDOB-UHFFFAOYSA-N 0.000 claims description 7
- 238000004587 chromatography analysis Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- 238000012937 correction Methods 0.000 claims description 4
- 230000004907 flux Effects 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 230000002000 scavenging effect Effects 0.000 claims description 4
- 230000009849 deactivation Effects 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 22
- 238000004458 analytical method Methods 0.000 abstract description 13
- 230000035945 sensitivity Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 238000011017 operating method Methods 0.000 abstract description 2
- 238000003908 quality control method Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 16
- 230000004044 response Effects 0.000 description 15
- 238000002203 pretreatment Methods 0.000 description 10
- 238000011084 recovery Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229960000583 acetic acid Drugs 0.000 description 7
- 239000000447 pesticide residue Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000012362 glacial acetic acid Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- -1 phonamiphos Chemical compound 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XJFIKRXIJXAJGH-UHFFFAOYSA-N 5-chloro-1,3-dihydroimidazo[4,5-b]pyridin-2-one Chemical group ClC1=CC=C2NC(=O)NC2=N1 XJFIKRXIJXAJGH-UHFFFAOYSA-N 0.000 description 3
- 239000005945 Chlorpyrifos-methyl Substances 0.000 description 3
- 235000009754 Vitis X bourquina Nutrition 0.000 description 3
- 235000012333 Vitis X labruscana Nutrition 0.000 description 3
- 240000006365 Vitis vinifera Species 0.000 description 3
- 235000014787 Vitis vinifera Nutrition 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 235000013402 health food Nutrition 0.000 description 3
- QXJKBPAVAHBARF-BETUJISGSA-N procymidone Chemical compound O=C([C@]1(C)C[C@@]1(C1=O)C)N1C1=CC(Cl)=CC(Cl)=C1 QXJKBPAVAHBARF-BETUJISGSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 241000026010 Dendrobium candidum Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- NDAUXUAQIAJITI-UHFFFAOYSA-N albuterol Chemical compound CC(C)(C)NCC(O)C1=CC=C(O)C(CO)=C1 NDAUXUAQIAJITI-UHFFFAOYSA-N 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000007717 exclusion Effects 0.000 description 2
- 238000001595 flow curve Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002917 insecticide Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 229960002052 salbutamol Drugs 0.000 description 2
- 238000002098 selective ion monitoring Methods 0.000 description 2
- 238000004885 tandem mass spectrometry Methods 0.000 description 2
- AMFGTOFWMRQMEM-UHFFFAOYSA-N triazophos Chemical compound N1=C(OP(=S)(OCC)OCC)N=CN1C1=CC=CC=C1 AMFGTOFWMRQMEM-UHFFFAOYSA-N 0.000 description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000218176 Corydalis Species 0.000 description 1
- 239000005946 Cypermethrin Substances 0.000 description 1
- JHJOOSLFWRRSGU-UHFFFAOYSA-N Fenchlorphos Chemical compound COP(=S)(OC)OC1=CC(Cl)=C(Cl)C=C1Cl JHJOOSLFWRRSGU-UHFFFAOYSA-N 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 240000008397 Ganoderma lucidum Species 0.000 description 1
- 235000001637 Ganoderma lucidum Nutrition 0.000 description 1
- 235000011201 Ginkgo Nutrition 0.000 description 1
- 235000008100 Ginkgo biloba Nutrition 0.000 description 1
- 244000194101 Ginkgo biloba Species 0.000 description 1
- 244000241872 Lycium chinense Species 0.000 description 1
- 235000015468 Lycium chinense Nutrition 0.000 description 1
- 231100000703 Maximum Residue Limit Toxicity 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- GXCLVBGFBYZDAG-UHFFFAOYSA-N N-[2-(1H-indol-3-yl)ethyl]-N-methylprop-2-en-1-amine Chemical compound CN(CCC1=CNC2=C1C=CC=C2)CC=C GXCLVBGFBYZDAG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 244000018633 Prunus armeniaca Species 0.000 description 1
- 235000009827 Prunus armeniaca Nutrition 0.000 description 1
- 239000005846 Triadimenol Substances 0.000 description 1
- QCJQWJKKTGJDCM-UHFFFAOYSA-N [P].[S] Chemical compound [P].[S] QCJQWJKKTGJDCM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003785 benzimidazolyl group Chemical group N1=C(NC2=C1C=CC=C2)* 0.000 description 1
- OMFRMAHOUUJSGP-IRHGGOMRSA-N bifenthrin Chemical compound C1=CC=C(C=2C=CC=CC=2)C(C)=C1COC(=O)[C@@H]1[C@H](\C=C(/Cl)C(F)(F)F)C1(C)C OMFRMAHOUUJSGP-IRHGGOMRSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KXRPCFINVWWFHQ-UHFFFAOYSA-N cadusafos Chemical compound CCC(C)SP(=O)(OCC)SC(C)CC KXRPCFINVWWFHQ-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229940125773 compound 10 Drugs 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229960005424 cypermethrin Drugs 0.000 description 1
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- FHIVAFMUCKRCQO-UHFFFAOYSA-N diazinon Chemical compound CCOP(=S)(OCC)OC1=CC(C)=NC(C(C)C)=N1 FHIVAFMUCKRCQO-UHFFFAOYSA-N 0.000 description 1
- BWUPSGJXXPATLU-UHFFFAOYSA-N dimepiperate Chemical compound C=1C=CC=CC=1C(C)(C)SC(=O)N1CCCCC1 BWUPSGJXXPATLU-UHFFFAOYSA-N 0.000 description 1
- MCWXGJITAZMZEV-UHFFFAOYSA-N dimethoate Chemical compound CNC(=O)CSP(=S)(OC)OC MCWXGJITAZMZEV-UHFFFAOYSA-N 0.000 description 1
- DOFZAZXDOSGAJZ-UHFFFAOYSA-N disulfoton Chemical compound CCOP(=S)(OCC)SCCSCC DOFZAZXDOSGAJZ-UHFFFAOYSA-N 0.000 description 1
- 230000000763 evoking effect Effects 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000012055 fruits and vegetables Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- NNKVPIKMPCQWCG-UHFFFAOYSA-N methamidophos Chemical compound COP(N)(=O)SC NNKVPIKMPCQWCG-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- KRTSDMXIXPKRQR-AATRIKPKSA-N monocrotophos Chemical compound CNC(=O)\C=C(/C)OP(=O)(OC)OC KRTSDMXIXPKRQR-AATRIKPKSA-N 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003987 organophosphate pesticide Substances 0.000 description 1
- 229960000490 permethrin Drugs 0.000 description 1
- RLLPVAHGXHCWKJ-UHFFFAOYSA-N permethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 RLLPVAHGXHCWKJ-UHFFFAOYSA-N 0.000 description 1
- BULVZWIRKLYCBC-UHFFFAOYSA-N phorate Chemical compound CCOP(=S)(OCC)SCSCC BULVZWIRKLYCBC-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000012224 working solution Substances 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some 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
- G01N2030/047—Standards external
Landscapes
- 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)
Abstract
The present invention relates to the detection method that agriculture is residual, a kind of disclose FaPEx GC MS/MS while detecting multi-tesidual pesticides in healthy food material method.The method includes the steps of：1）Pretreatment；2）Purification；3）Preparing standard solution；4）Detection.The present invention uses extracting process appropriate and FaPEx column purifications, simultaneously to GC MS/MS condition optimizings, detection speed is fast, under the premise of ensureing that accuracy, repeatability, sensitivity etc. meet the requirement of retention analysis quality control guide, its operating procedure is easy, preferably eliminates matrix effect.Reduce the pollution level to instrument, extend instrument service life, support is provided for the remaining detection of pesticide in current healthy food material and safety evaluatio.
Description
Technical field
The present invention relates to the residual detection method of agriculture more particularly to a kind of FaPEx-GC-MS/MS to detect health food original simultaneously
The method of multi-tesidual pesticides in material.
Background technology
In the Multi-residue analysis of healthy food material, complicated variety (fat, pigment, the carbohydrate of matrix components
And some insoluble impurities etc.), it is similar to the structure of certain pesticides and property, it is easier to interference phenomenon occur；Additionally, it is possible to institute
Some volatile compounds contained easily interfere trace analysis, and detection limit of many pesticides in healthy food material is very high
Can not even detect so that there are still larger uncertainties for trace residue object qualitative, quantitative in complex matrices, therefore to its
Multi-residue analysis is always the difficulties in farming residual analysis field.
QuEChERS methods are the detection means of the pesticide residue generally used both at home and abroad at present, but its step is comparatively
Complexity, and its exothermic phenomenon causes low boiling point object to be degraded；The addition of ketjenblack EC so that the pesticide of flat annular is dividing
Dissipate in matrix extraction by strong adsorption, these factors affects to result it is accurate whether.Matrix effect detects agriculture in vapor phase method
It is inevitable in residual, matrix effect problem can not be fully solved using multiple purifying method, especially with sample preparation steps
Increase, pre-treatment cost and time will all increase.
Sample purification when disclosing a kind of detection for fruit and vegetable residual pesticide application No. is 201710089362.6 Chinese patent
Adsorbent, sample-pretreating method and the residual detection method of agriculture, the purifying adsorbent provided for garden stuff pesticide residue when detecting
When sample pre-treatments, to effectively shorten time of pre-treatment, detection can be improved to avoid the multiple centrifugation in pretreatment process
Accuracy rate.But this method adsorbent preparation process is complicated, and it is easy absorption substance to be checked, testing result is influenced, also can not
Solve the problems, such as matrix effect.
Invention content
In order to solve the above technical problem, the present invention provides a kind of FaPEx-GC-MS/MS to detect health food original simultaneously
The method of multi-tesidual pesticides in material, using extracting process appropriate and FaPEx column purifications, and meanwhile it is excellent to GC-MS/MS conditions
Change, detection speed is fast, has the higher rate of recovery and precision, reduces the pollution to instrument, and improve instrument uses the longevity
Life.
The specific technical solution of the present invention is：The method includes the steps of：
1) it pre-processes：Addition acetate acetonitrile solution obtains mixed liquor after weighing healthy food material homogeneous；
2) it purifies：Mixed liquor is crossed into FaPEx columns and obtains scavenging solution；
3) preparing standard solution：The acetone soln of pesticide and matrix matching liquid is configured to series concentration by gradient dilution
Standard solution；
4) it detects：Scavenging solution is measured using GC-MS/MS methods, is confirmed according to the retention time of different agricultural chemical compounds and is examined
Go out compound, agricultural chemical compound content is determined according to multiple-reaction monitoring pattern (MRM) method and standard solution.
It is important due to being had to pesticide extraction in healthy food material by the selection of pesticide polarity effect, extracting and purifying solvent
It influences, acetonitrile is more preferable compared with other solvents to the dissolubility of most pesticides, and the introducing of a small amount of acetic acid can form buffer body
System reduces influence of the matrix solution acid-base property to extraction, to increase the extraction efficiency of pesticide.
Healthy food material is mostly various Chinese medicines and animal and plant extracts, such as dendrobium candidum, lucidum spore powder, Agricus blazei
Deng, complicated component is various (fat, pigment, carbohydrate and some insoluble impurities etc.), and with the structure of certain pesticides, property
It is similar, not only easily there is interference phenomenon, fatal damage can be also caused to chromatographic column and mass spectrum, it is necessary to matrix is purified,
The present invention purifies matrix using FaPEx columns, and the rate of recovery and stability are high, and the pre-treatment time is short, without repeatedly extraction, from
The heart, purification process, which takes, only needs about 30s, easy to operate, saves a large amount of manpower and materials.
For the pesticide of same concentrations, the chromatography response in matrix solution can be higher than its response in pure solvent.
To certain a sample it is quantitative when, using the bare substrate sample carry out configuration standard solution, the influence of matrix effect can be eliminated,
So that testing result accuracy and repeatability reach requirement.
By right《Chinese Pharmacopoeia》Specified in the detection method of 76 kinds of pesticides and its residual quantity in medicinal material, medicine materical crude slice and preparation
Analysis, not only its step is relatively complicated for general QuEChERS methods, pre-treatment needs take a long time, not only need
A large amount of organic solvent is wanted, and more pre-treatment be easy to cause the risk of pesticide loss, influences the rate of recovery, does not meet nowadays
The requirement quickly detected, since surveyed pesticide is largely volatile compounds, GC-MS/MS methods are that detection health food is former
More optimum detection methods of pesticide residue in material, sensitivity is higher, and fast and convenient, but gas-chromatography wants sample
Ask higher, if sample purification degree not enough easily pollutes instrument or blocks, and the great challenge of more Residual insecticides
The reason of also reside under low-down MRL values ppb concentration level sensitivity, which is wanted, to be realized to nearly hundred kinds of pesticides in complex matrices
The detection limit asked, the sample analysis in being controlled also for regular quality, sample pre-treatments should simplify, and avoid tedious steps.
And for healthy food material, all have due to the complicated variety of its matrix, and for most agricultural chemical compounds
There is volatility, and there is also differences for the polarity power of compound, therefore the selection of sample pre-treatments is not only related to analysis result
Accuracy, and be related to the sample into instrument to pollution level caused by instrument itself.The present invention by adjusting extraction,
Reagent, operation and the parameter of purification and detection combine FaPEx column purifications method and GC-MS/MS methods, time-consuming very short, total to try
Agent only needs 3-5min, accuracy in detection and precision also to increase compared with other methods, detection pesticide variety from《China
Pharmacopeia》Defined 76 kinds increase to 95 kinds.
The foundation of GC-MS/MS methods is in the detection of multi-pesticide residue, using multiple-reaction monitoring pattern (MRM) than single level Four
Salbutamol Selected Ion Monitoring pattern (SIM) exclusion background interference ability is stronger, and specificity is stronger, can enhance the reliable of qualitative results
Property, and due to it is quantitative when background values substantially reduce, to make the sensitivity of detection be greatly improved.
Preferably, acetate acetonitrile solution concentration is 0.9-1.1wt% in the step 1), solution is with material quality ratio
5∶0.9-1.1。
Influence by Experimental comparison's difference glacial acetic acid ratio to extraction efficiency, it is found that when glacial acetic acid is 1wt% or so, absolutely
The rate of recovery of most of pesticide is with respect to highest.
Preferably, acetonitrile is the acetonitrile being saturated by n-hexane in the step 1).
For high-water content matrix sample, acetonitrile miscible with water can cause to remove water in subsequent experimental in Extraction solvent
Difficulty reduces the polarity of its Extraction solvent therefore, it is necessary to which acetonitrile to be saturated by n-hexane, alleviates the pressure subsequently removed water.
Preferably, also needing acutely to shake 20-40 seconds after acetate acetonitrile solution is added in the step 1), then stand 50-
70s。
Preferably, specific purification process is that mixed liquor is poured into FaPEx columns in the step 2), with 1 drip per second speed
Pressurization, takes the filtrate nitrogen of certain volume to dry up, then be settled to original volume with acetone.
Mixed liquor, which spends the FaPEx column times, only needs 30s or so, takes very short.
Since the polarity of different pesticides itself has differences, solubility in a solvent directly influences the sound on instrument
It should be worth, finally determine its detection limit, present invention discover that in healthy food material system, using acetone solvent, each compound
Response it is high.
Preferably, step 3) the mesostroma matching fluid be with identical preprocess method and FaPEx columns treated sky
White matrix sample.
Preferably, chromatography (GC) operating condition is the HP-5MS UI (μ of 30m × 0.25mm × 0.25 in the step 4)
m)；Bushing pipe：Agilent 5190-2293 (deactivation, 900 μ L, do not shunt)；Injector temperature：280V；Dottle pin purge flow rate：
3mL/min；Column oven temperature program：60 DEG C (1min) is warming up to 120 DEG C with 40 DEG C/min and is warming up to 310 DEG C again with 5 DEG C/min；
Carrier gas：Helium (purity ＞ 99.9995%), constant voltage mode：7.9psi；Sample size：1μL；Input mode：Splitless injecting samples,
Flow divider is opened after 1min.After run 5min, column oven temperature：310℃.
Preferably, mass spectrum (MS) operating condition is electron impact ionization source (EI) 70eV in the step 4)；Ion source
280 DEG C of temperature；280 DEG C of transmission line temperature；35~400amu of scanning of the mass spectrum range；Solvent delay time 3min.
Preferably, MRM establishes 8 periods in the step 4).
Preferably, the retention time of different agricultural chemical compounds is controlled by EPC under constant voltage mode in the step 4)
Pressing pressure adjusts carrier gas flux, establishes flow velocity and the correction relationship of pressure so that retention time is restored to preset state, realizes
Retention time locks.
Due in gas-chromatography column temperature, flow rate of carrier gas, the chemical property of fixer and stability, (packed column) carrier or
The factors such as the chemical property of glass tube walls have an impact retention, and the retention of different experimental determinations also tends to not
Together.Therefore retention time locking will be much easier for the identification at peak.The present invention is controlled by EPC and is pressed under constant voltage mode
Power adjusts carrier gas flux, establishes flow velocity and the correction relationship of pressure so that retention time is restored to preset state, realizes and retains
Time lock.The retention time of sample and reference substance is set to be slightly different in different time, different location, certain instrumentation conditions
When remain unchanged, to easily identifying unknown material.
It is compared with the prior art, the beneficial effects of the invention are as follows：The present invention is net using extracting process appropriate and FaPEx columns
Change, while to GC-MS/MS condition optimizings, detection speed is fast, meets retention analysis in guarantee accuracy, repeatability, sensitivity etc.
Under the premise of the requirement of quality control guide, operating procedure is easy, preferably eliminates matrix effect.Reduce the dirt to instrument
Dye degree extends instrument service life, and branch is provided for the remaining detection of pesticide in current healthy food material and safety evaluatio
It holds.
Description of the drawings
Fig. 1 is the chlorpyrifos-methyl RTlock Pressure-flow curves figures of the present invention；
Fig. 2 is the TIC figures of 95 kinds of pesticide standard solution (500ng/mL) of the present invention.
Specific implementation mode
With reference to embodiment, the invention will be further described.
1. experimental section
1.1 instruments and reagent
1 key instrument list of table
Reagent：Acetone, acetonitrile, toluene are chromatographically pure (German Merck companies), and glacial acetic acid is AR analysis levels (traditional Chinese medicines collection
Chemical reagent Co., Ltd of group), standard sample of pesticide is purchased from Beijing Tan Mo quality inspections Science and Technology Ltd., and purity is 99% or more.
The operating condition of 1.2 instruments
Chromatographic condition：HP-5MS UI(30m×0.25mm×0.25μm)；Bushing pipe：Agilent 5190-2293 (deactivations
Property, 900 μ L are not shunted)；Injector temperature：280V；Dottle pin purge flow rate：3mL/min；Column oven temperature program：60℃
(1min) is warming up to 120 DEG C with 40 DEG C/min and is warming up to 310 DEG C again with 5 DEG C/min；Carrier gas：Helium (purity ＞ 99.9995%),
Constant voltage mode：7.9psi；Sample size：1μL；Input mode：Splitless injecting samples open flow divider after 1min.After run 5min, column
Temperature of Warm Case：310℃.
Mass Spectrometry Conditions：Electron impact ionization source (EI) 70eV；280 DEG C of ion source temperature；280 DEG C of transmission line temperature；Mass spectrum
35~400amu of scanning range；Solvent delay time 3min.MRM conditions are separately optimized according to different pesticides, relevant parameter
It is shown in Table 2.95 kinds of agricultural chemical compound TIC figures are shown in Fig. 1.
The configuration of 1.3 standard solution
Standard reserving solution：Suitable standard mother liquor is accurately drawn respectively, and the pesticide that 10 μ g/mL are diluted to acetone mixes
Standardization storing solution is preserved in 0~4 DEG C of refrigerator.
Standard solution：Appropriate pesticide standard stock solution is accurately drawn, according to the sensitivity of each agricultural chemical compound and instrument
The device range of linearity draws a certain amount of pestsides synthesis standard reserving solution, passes through gradient with the acetone reagent containing matrix matching liquid
Dilution is configured to the matrix hybrid standard working solution of series concentration.
1.4 sample pre-treatments
Sample after about 1g homogeneous is weighed, the 1% acetate acetonitrile solution of 5mL is added, acutely concussion 30 seconds, stands 1min,
Enter FaPEx extraction columns, pressurizeed (about 30 seconds) with 1 drip speed per second, takes 1mL nitrogen to be blown to close dry, 1mL is settled to acetone, for GC-
MS/MS is analyzed.
2 results and discussion
The foundation of 2.1GC-MS/MS methods
2.1.1 retention time locks
Qualitative always of people's attention problem of the unknown compound in chromatography.In mass spectral analysis, protected using chromatography
It is the current most reliable method for carrying out qualitative analysis to stay value to be combined with Information in Mass Spectra.Due to the column temperature in gas-chromatography, carrier gas
The factors such as the chemical property of flow velocity, the chemical property of fixer and stability, (packed column) carrier or glass tube walls are to retention
Have an impact, and the retention of different experimental determinations also tends to difference.Therefore retention time locks the identification for peak
It will be much easier.The present invention adjusts carrier gas flux by EPC control pressures, establishes flow velocity and pressure under constant voltage mode
Correction relationship so that retention time is restored to preset state, realizes the locking of chlorpyrifos-methyl retention time.Make sample and standard
The retention time of object is remained unchanged when different time, different location, certain instrumentation conditions are slightly different, to easily
The retention time data base for establishing identification unknown material carries out unknown sample according to the database simple qualitative.Fig. 1 is methyl poison
Dead tick Pressure-flow curves finally lock it in 18.11min by being corrected to chlorpyrifos-methyl RTlock.
2.1.2MRM method is established
The foundation of GC-MS/MS methods is in the detection of multi-pesticide residue, using multiple-reaction monitoring pattern (MRM) than single level Four
Salbutamol Selected Ion Monitoring pattern (SIM) exclusion background interference ability is stronger, and specificity is stronger, can enhance the reliable of qualitative results
Property, and due to it is quantitative when background values substantially reduce, to make the sensitivity of detection be greatly improved.This experiment is according to 95 kinds
The actual conditions of agricultural chemical compound establish 8 periods, and each period according to the property of compound, adjusts residence time,
Select the ion that abundance is high, not disturbed as daughter ion；By optimizing collision energy, final foundation is accurate qualitative, quantitative
MRM methods, are specifically shown in Table 1.
The optimization of 2.2 extraction and cleaning conditions
It is important due to being had to pesticide extraction in healthy food material by the selection of pesticide polarity effect, extracting and purifying solvent
It influences, acetonitrile is more preferable compared with other solvents to the dissolubility of most pesticides, and the introducing of a small amount of acetic acid can form buffer body
System reduces influence of the matrix solution acid-base property to extraction, to increase the extraction efficiency of pesticide.By comparing different glacial acetic acid matter
Influence of the ratio (0,0.5%, 1%, 3%) to extraction efficiency is measured, finds the recycling of overwhelming majority pesticide when glacial acetic acid is 1wt%
Rate is with respect to highest.In fact, because sample preparation steps increase the analysis throughput that can reduce sample with the increase of complexity,
And the accuracy for also influencing method is also that it obtains the premise of satisfactory result because this extraction and purification methods is simple and efficient.
It is worth noting that, for high-water content matrix sample, after acetonitrile miscible with water can cause in Extraction solvent
The difficulty removed water in continuous experiment reduces the polarity of its Extraction solvent, alleviates therefore, it is necessary to which acetonitrile to be saturated by n-hexane
The pressure subsequently removed water.
In addition, since the polarity of different pesticides itself has differences, solubility in a solvent is directly influenced in instrument
On response, finally determine its detection limit.Most widely used solvent is acetone, acetonitrile, toluene etc. in the analysis of agricultural drugs, is passed through
Experimental result shows, other two kinds of solvents are compared using acetone, and the response of each compound is high, therefore using acetone as molten
Agent.
2.3 matrix effect
For the pesticide of same concentrations, the chromatography response in matrix solution can be higher than its response in pure solvent.
Ideally, to certain a sample it is quantitative when, using the bare substrate sample carry out configuration standard solution, matrix can be eliminated
The influence of effect so that testing result accuracy and repeatability reach requirement.Erney etc. proposes the response enhancing of matrix inducing color chromatogram
Phenomenon caused extensive dispute in scientific circles at that time.By the decomposition of the reduction thermally labile pesticide in vaporescence, and
Active site in shielding injection port and reduce the speed of absorption and desorption of the polarity pesticide in active site, sample substrate increases
Transmission quantity of the pesticide to be analyzed from injection port to chromatographic column.Experiment finds that two class compounds are also easy to produce matrix enhancement effect, one
Class is the compound of thermally labile at the vaporization temperature, and one kind is the chemical combination easily adsorbed when sample enters chromatographic column or detector
Object.By compared with pure solvent standard solution, it may be said that the bright pesticide rate of recovery sensitive to the enhancing of matrix evoked response, which increases, is
Due to the protective effect of matrix.The real response value of pure solvent standard solution should enter the value that chromatographic column generates less than it,
It is because pure solvent cannot provide enough protections for pesticide to be analyzed, and add the agriculture of same concentrations in vehicle solution
Medicine can be such that pesticide is more fully transferred in chromatographic column, increase to respond, and matrix plays analysis and protects in this process
Shield acts on.
95 kinds of agricultural chemical compounds are used pure acetone and handle the Agricus blazei bare substrate sample obtained with FaPaX by the present invention respectively
Product are configured to the standard solution of a concentration of 10ng/mL, 100ng/mL, 200ng/mL, and the TIC figures of standard solution are shown in Fig. 2, pass through survey
Set the goal average response value (A, n=3) of the object in pure acetone and average response value (B, the n=in matrix matching standard solution
3) matrix effect (Matrix Effect, ME)=B/A, is obtained.
Statistics indicate that the same pesticide compound of various concentration and the different agricultural chemical compounds of same concentration, matrix
Effect all has differences；But for most agricultural chemical compounds, concentration is proportionate with its matrix effect, for big absolutely
Most agricultural chemical compounds, the addition of matrix, which can enhance, even largely enhances response of the target compound on instrument.
The result shows that the typical pesticides of matrix effect sensitivity have：Biphenthrin, Permethrin, basudin, Rogor, disulfoton, horse traction sulphur
Phosphorus, acephatemet, Azodrin, Hostathion, cadusafos, thimet, Hostathion, phonamiphos, Triadimenol, chlopyrifos, Nankor, triazole
Ketone, procymidone, different rice blast net etc..This kind of pesticide has polarity mostly or can form the acid or alkaline chemical combination of strong hydrogen bonding effect
Object generally carries phosphate (- P=O), hydroxyl, amino, imidazole radicals, benzimidazolyl, carbamate groups (- O-CO-NH-)
With urea groups (- NH-CO-NH-) functional group.In addition, the organophosphorus pesticide with-P=S groups compares the organophosphor of-P=O groups
Pesticide, being influenced by matrix effect can be smaller.
2.4 methodological study
Although matrix components can cause pesticide, response greatly increases, and is desirable to be obtained with minimum matrix in practice
Stable matrix enhancement effect.Therefore, preferable pre-treatment should reach rational sample purification, and only need instrument system appropriate
System is safeguarded.The present invention uses FaPEx column Rapid Extraction purification techniques, adds 95 kinds of pesticides of different content level in the sample,
Extraction standard solution is prepared with bare substrate extract liquor and compensates matrix effect, and every group of replication 3 times calculates returning for various pesticides
Yield and relative standard deviation SRD values.Under the low concentration of 10ppb, part of compounds is not detected, but the high concentration of 100ppb
Under, except Bravo is not detected, the average recovery rate of other 94 kinds of agricultural chemical compounds only has 2 and is less than 75%, remaining exists
76.3%~156.0%, RSD value ranging from 0.3%~15.4%, the RDS values of 90% or more agricultural chemical compound 10% with
Under, specifically it is shown in Table 2.Accuracy and precision reach the requirement of pesticide residue analysis.When with gas chromatography determination sample,
Sample mesostroma ingredient reduces the decomposition of heat-labile compound in injection port gasification, shields the activity of injection port
Site so that the bonding machine of target compound and active site can greatly reduce, and increases component to be measured and enters chromatography
Transmission quantity in column so that the response of target compound is different.Matrix matching standard solution is used in more Residual insecticides
External standard method, which is calibrated, quantitatively can preferably compensate matrix effect.Therefore, 5 differences are configured in the 5-500ng/mL ranges of linearity
The mixed standard solution of mass concentration gradient, using peak area Y as ordinate, mass concentration is abscissa, and it is bent to draw standard work
Line after least square method quadratic fit, obtains preferable linearity curve and closes to 18 kinds of agricultural chemical compounds such as cypermethrin
System.Specifically it is shown in Table 3.
The result shows that：In the range of investigated, 95 kinds of pesticides can obtain the comparatively ideal rate of recovery and relative standard is inclined
Difference, this method meet requirement of the detection method to precision, and detection lower bound meets various countries' limitation requirement.
2 95 kinds of pesticide retention times of table, collision ion, related coefficient (r2), quantitative limit, the rate of recovery and relative standard it is inclined
Poor (n=3)
3 95 kinds of agricultural chemical compound linearity curves of table
3. specific implementation
Detection method using the present invention is in grape pip, ginkgo leaf, apricot skin, dendrobium candidum, the fruit of Chinese wolfberry, Rhizoma Atractylodis Macrocephalae, stir-fry
The measurement of chicken gold, coloured malt, corydalis tuber, ganoderma lucidum, Agricus blazei totally 11 kinds of healthy food materials does two parallel places per class raw material
Reason measures three times every group of processing, is averaged.It is as shown in table 4 below to test acquired results, is not difficult to find out, for institute's sample
All there is a certain amount of pesticide residue in product, detection value is higher wherein in grape pip dimepiperate, procymidone, GB/T2763-
2014 define the maximum residue limit for allowing all kinds of pesticides in food, and standard provides that the residual limitation of the agriculture in vegetable and fruit is minimum and reaches
0.01mg/kg.And it uses《Chinese Pharmacopoeia》Defined QuEChERS methods detect above-mentioned 11 kinds of healthy food materials, gained detection
As a result in, such as the higher pesticide of some persticide residues of procymidone is detected in grape pip, but residual quantity is than the present invention
It is relatively low or consistent with the present invention, but there is no evident regularities, and some present invention of phonamiphos detect in such as Rhizoma Atractylodis Macrocephalae but pesticide is residual
Stay lower pesticide undetected.
Pesticide determined result of residue in 4 11 kinds of healthy food materials of table
Note：ND expressions are not detected.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit still falls within the technology of the present invention side to any simple modification, change and equivalent transformation made by above example
The protection domain of case.
Claims (10)
1. a kind of method that FaPEx-GC-MS/MS detects multi-tesidual pesticides in healthy food material simultaneously, which is characterized in that
The method includes the steps of：
1）Pretreatment：Addition acetate acetonitrile solution obtains mixed liquor after weighing healthy food material homogeneous；
2）Purification：Mixed liquor is crossed into FaPEx columns and obtains scavenging solution；
3）Preparing standard solution：The acetone soln of pesticide and matrix matching liquid is configured to the mark of series concentration by gradient dilution
Quasi- solution；
4）Detection：Scavenging solution is measured using GC-MS/MS methods, detectionization is confirmed according to the retention time of different agricultural chemical compounds
Object is closed, according to multiple-reaction monitoring pattern（MRM）Method and standard solution determine agricultural chemical compound content.
2. FaPEx-GC-MS/MS as described in claim 1 detects the side of multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 1）Middle acetate acetonitrile solution concentration is 0.9-1.1wt%, and solution is 5 with material quality ratio:
0.9-1.1。
3. FaPEx-GC-MS/MS as claimed in claim 1 or 2 detects multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 1）Middle acetonitrile is the acetonitrile being saturated by n-hexane.
4. FaPEx-GC-MS/MS as claimed in claim 1 or 2 detects multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 1）It also needs acutely to shake 20-40 seconds after middle addition acetate acetonitrile solution, then stands 50-
70s。
5. FaPEx-GC-MS/MS as described in claim 1 detects the side of multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 2）In specific purification process be that mixed liquor is poured into FaPEx columns, added with 1 drip speed per second
Pressure, takes the filtrate nitrogen of certain volume to dry up, then be settled to original volume with acetone.
6. FaPEx-GC-MS/MS as described in claim 1 detects the side of multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 3）Mesostroma matching fluid is with identical preprocess method and FaPEx columns treated blank base
Quality sample.
7. FaPEx-GC-MS/MS as described in claim 1 detects the side of multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 4）Middle chromatography（GC）Operating condition is HP-5MS UI (30m × 0.25mm × 0.25 μm)；Lining
Pipe：Agilent 5190-2293 (deactivation, 900 μ L, do not shunt)；Injector temperature：280 V；Dottle pin purge flow rate：3mL/
min；Column oven temperature program：60 DEG C (1min) is warming up to 120 DEG C with 40 DEG C/min and is warming up to 310 DEG C again with 5 DEG C/min；It carries
Gas：Helium (purity ＞ 99.9995%), constant voltage mode：7.9psi；Sample size：1μL；Input mode：Splitless injecting samples, after 1min
Flow divider is opened, runs 5min, column oven temperature afterwards：310℃.
8. FaPEx-GC-MS/MS as claimed in claim 1 or 7 detects multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 4）Middle mass spectrum（MS）Operating condition is electron impact ionization source（EI）70eV；Ion source temperature
280 DEG C of degree；280 DEG C of transmission line temperature；35 ~ 400amu of scanning of the mass spectrum range；Solvent delay time 3min.
9. FaPEx-GC-MS/MS as claimed in claim 8 detects the side of multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 4）Middle MRM establishes 8 periods.
10. FaPEx-GC-MS/MS as claimed in claim 1 or 7 detects multi-tesidual pesticides in healthy food material simultaneously
Method, which is characterized in that the step 4）The retention time of middle difference agricultural chemical compound is controlled by EPC under constant voltage mode
Pressing pressure adjusts carrier gas flux, establishes flow velocity and the correction relationship of pressure so that retention time is restored to preset state, realizes
Retention time locks.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810378346.3A CN108572225A (en) | 2018-04-25 | 2018-04-25 | A kind of method that FaPEx-GC-MS/MS detects multi-tesidual pesticides in healthy food material simultaneously |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810378346.3A CN108572225A (en) | 2018-04-25 | 2018-04-25 | A kind of method that FaPEx-GC-MS/MS detects multi-tesidual pesticides in healthy food material simultaneously |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108572225A true CN108572225A (en) | 2018-09-25 |
Family
ID=63575186
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810378346.3A Pending CN108572225A (en) | 2018-04-25 | 2018-04-25 | A kind of method that FaPEx-GC-MS/MS detects multi-tesidual pesticides in healthy food material simultaneously |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108572225A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696487A (en) * | 2019-02-14 | 2019-04-30 | 罗俊霞 | Because of the modification method of analysis result error caused by matrix effect in instrument analysis |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102645498A (en) * | 2012-05-22 | 2012-08-22 | 中国烟草总公司贵州省公司 | Method for detecting residues of 202 pesticides in tobacco leaves |
| CN103472155A (en) * | 2013-09-29 | 2013-12-25 | 邬金飞 | Gas chromatographic method for detecting residue amount of nine kinds of organophosphorus pesticide in rice |
| CN103512993A (en) * | 2013-10-12 | 2014-01-15 | 崔淑华 | Hot pepper and determining method for 96 pesticide residues in product of hot pepper |
| CN105486795A (en) * | 2015-12-28 | 2016-04-13 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technique for 708 pesticide residues in berries and other small fruits |
| CN106896176A (en) * | 2017-03-21 | 2017-06-27 | 舟山出入境检验检疫局综合技术服务中心 | A kind of method of unknown residues of pesticides in non-targeted rapid screening import Cereals of FaPEx UPLC Q TOF |
| CN106918668A (en) * | 2015-12-28 | 2017-07-04 | 天士力制药集团股份有限公司 | The detection method of Yixinfumai particle Pesticide Residues |
-
2018
- 2018-04-25 CN CN201810378346.3A patent/CN108572225A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102645498A (en) * | 2012-05-22 | 2012-08-22 | 中国烟草总公司贵州省公司 | Method for detecting residues of 202 pesticides in tobacco leaves |
| CN103472155A (en) * | 2013-09-29 | 2013-12-25 | 邬金飞 | Gas chromatographic method for detecting residue amount of nine kinds of organophosphorus pesticide in rice |
| CN103512993A (en) * | 2013-10-12 | 2014-01-15 | 崔淑华 | Hot pepper and determining method for 96 pesticide residues in product of hot pepper |
| CN105486795A (en) * | 2015-12-28 | 2016-04-13 | 中国检验检疫科学研究院 | GC-Q-TOF/MS detection technique for 708 pesticide residues in berries and other small fruits |
| CN106918668A (en) * | 2015-12-28 | 2017-07-04 | 天士力制药集团股份有限公司 | The detection method of Yixinfumai particle Pesticide Residues |
| CN106896176A (en) * | 2017-03-21 | 2017-06-27 | 舟山出入境检验检疫局综合技术服务中心 | A kind of method of unknown residues of pesticides in non-targeted rapid screening import Cereals of FaPEx UPLC Q TOF |
Non-Patent Citations (5)
| Title |
|---|
| NASIRI, A 等: "A Multi Residue GC-MS Method for Determination of 12 Pesticides in Cucumber", 《IRANIAN JOURNAL OF PHARMACEUTICAL RESEARCH》 * |
| 农业药物毒物试验所: "《https://www.tactri.gov.tw/Uploads/Item/e26773db-8753-499b-bbfb-b21d89c337d4.pdf》", 1 January 2018 * |
| 国家食品药品监督管理总局科技和标准司: "《食品补充检验方法实操指南》", 28 February 2018, 中国医药科技出版社 * |
| 蒋施 等: "气相色谱-三重四级杆串联质谱法确证姜中120种农药残留量", 《农药》 * |
| 马永龙: "保健食品中主要化学危害物质检测技术研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109696487A (en) * | 2019-02-14 | 2019-04-30 | 罗俊霞 | Because of the modification method of analysis result error caused by matrix effect in instrument analysis |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106483232A (en) | The method for quick of Multiple Pesticides residual in a kind of soil | |
| CN108061768A (en) | A kind of structure and its detection method of Radix Paeoniae Alba HPLC characteristic spectrums | |
| CN105651899A (en) | Method for high-sensitivity detection of aflatoxin and application of aflatoxin | |
| CN107782835B (en) | A kind of method of efficient liquid phase detection fleabane flower ingredient | |
| CN108181397A (en) | Hangzhou chili capsaicine concentration extraction measuring method | |
| CN106353418A (en) | Method for simultaneously measuring 28 kinds of pesticide residues with gas chromatography-triple quadrupole tandem mass spectrometry | |
| Fan et al. | Design and application of Hadamard-injectors coupled with gas and supercritical fluid sample collection systems in Hadamard transform-gas chromatography/mass spectrometry | |
| CN105548431B (en) | Detect the method for oxamyl and oxamyl oxime residual quantity in vegetables/fruit simultaneously | |
| CN111089916B (en) | Method for detecting content of paeoniflorin, liquiritin and ammonium glycyrrhizinate in radix bupleuri and radix paeoniae alba oral liquid | |
| CN108572225A (en) | A kind of method that FaPEx-GC-MS/MS detects multi-tesidual pesticides in healthy food material simultaneously | |
| CN108614052B (en) | Method for simultaneously detecting gelsemine, gelsemine and gelsemine in biological sample based on two-dimensional liquid chromatography | |
| CN109709233A (en) | A method of a variety of mushroom toxin in detection blood, urine | |
| CN106053634A (en) | Method for detecting N-dimethyl nitrosamine in cooked meat products | |
| CN109765322A (en) | The characteristic spectrum construction method and quality determining method of schizonepeta | |
| CN109521106A (en) | Method that is a kind of while detecting four kinds of component contents in five composition granule of Radix Astragali ramulus cinnamomi | |
| CN113390997A (en) | Method for simultaneously and quantitatively detecting matrine and oxymatrine in tea | |
| CN104597189A (en) | Determining method of Pyrifluquinazon residual quantity | |
| CN110031564B (en) | Quality detection method of natural plant anticoccidial feed additive based on HPLC fingerprint | |
| CN110441413A (en) | The construction method and detection method of qianbai biyan tablets HPLC finger-print | |
| CN114216980B (en) | Method for establishing HPLC-ELSD fingerprint of starwort root | |
| CN106226433A (en) | The assay method of tilmicosin residue amount in a kind of florfenicol solution | |
| CN108226370A (en) | A kind of discriminating of traditional Chinese medicine gel and content assaying method | |
| Vink et al. | Simplified method for determination of the tetracyclic antidepressant mianserin in human plasma using gas chromatography with nitrogen detection | |
| CN107102078A (en) | A kind of method of aflatoxin B1 in measure Gardenia Yellow | |
| CN102539600A (en) | Method for detecting aminobutyric acid in sample by high efficiency liquid chromatography |
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: 20180925 |
|
| RJ01 | Rejection of invention patent application after publication |