CN115902066A - Method for detecting various pesticide residues in pseudo-ginseng - Google Patents
Method for detecting various pesticide residues in pseudo-ginseng Download PDFInfo
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- 235000003181 Panax pseudoginseng Nutrition 0.000 title claims abstract description 67
- 244000131316 Panax pseudoginseng Species 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 52
- 150000002500 ions Chemical class 0.000 claims abstract description 40
- 239000000575 pesticide Substances 0.000 claims abstract description 37
- 238000000605 extraction Methods 0.000 claims abstract description 31
- 238000001819 mass spectrum Methods 0.000 claims abstract description 26
- 230000014759 maintenance of location Effects 0.000 claims abstract description 12
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 50
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 36
- 239000012071 phase Substances 0.000 claims description 35
- 239000000243 solution Substances 0.000 claims description 35
- 238000004949 mass spectrometry Methods 0.000 claims description 31
- 230000005686 electrostatic field Effects 0.000 claims description 29
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 26
- 238000005185 salting out Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- 238000010828 elution Methods 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 15
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 13
- 235000019253 formic acid Nutrition 0.000 claims description 13
- 230000010355 oscillation Effects 0.000 claims description 13
- 238000001195 ultra high performance liquid chromatography Methods 0.000 claims description 13
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000008346 aqueous phase Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 239000012024 dehydrating agents Substances 0.000 claims description 11
- 239000012074 organic phase Substances 0.000 claims description 11
- 239000012488 sample solution Substances 0.000 claims description 11
- PYYLURXQRGDDCC-UHFFFAOYSA-N C(=O)O.C(=O)[O-].[NH4+].CO Chemical group C(=O)O.C(=O)[O-].[NH4+].CO PYYLURXQRGDDCC-UHFFFAOYSA-N 0.000 claims description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- ADCGAPKUMAQOLJ-UHFFFAOYSA-N azane;formic acid Chemical compound N.OC=O.OC=O ADCGAPKUMAQOLJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004445 quantitative analysis Methods 0.000 claims description 10
- 239000012629 purifying agent Substances 0.000 claims description 9
- 229960000583 acetic acid Drugs 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 3
- 239000002516 radical scavenger Substances 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims 1
- 238000004704 ultra performance liquid chromatography Methods 0.000 claims 1
- 238000003260 vortexing Methods 0.000 claims 1
- 235000003143 Panax notoginseng Nutrition 0.000 abstract description 10
- 241000180649 Panax notoginseng Species 0.000 abstract description 10
- 239000012634 fragment Substances 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000012216 screening Methods 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 3
- 239000002207 metabolite Substances 0.000 abstract description 2
- 238000002414 normal-phase solid-phase extraction Methods 0.000 abstract description 2
- 229940126680 traditional chinese medicines Drugs 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000011159 matrix material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000005760 Difenoconazole Substances 0.000 description 4
- 239000005842 Thiophanate-methyl Substances 0.000 description 4
- BQYJATMQXGBDHF-UHFFFAOYSA-N difenoconazole Chemical compound O1C(C)COC1(C=1C(=CC(OC=2C=CC(Cl)=CC=2)=CC=1)Cl)CN1N=CN=C1 BQYJATMQXGBDHF-UHFFFAOYSA-N 0.000 description 4
- UWVQIROCRJWDKL-UHFFFAOYSA-N oxadixyl Chemical compound CC=1C=CC=C(C)C=1N(C(=O)COC)N1CCOC1=O UWVQIROCRJWDKL-UHFFFAOYSA-N 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 4
- QGHREAKMXXNCOA-UHFFFAOYSA-N thiophanate-methyl Chemical compound COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC QGHREAKMXXNCOA-UHFFFAOYSA-N 0.000 description 4
- QNBTYORWCCMPQP-JXAWBTAJSA-N (Z)-dimethomorph Chemical compound C1=C(OC)C(OC)=CC=C1C(\C=1C=CC(Cl)=CC=1)=C/C(=O)N1CCOCC1 QNBTYORWCCMPQP-JXAWBTAJSA-N 0.000 description 3
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 description 3
- 239000005761 Dimethomorph Substances 0.000 description 3
- 239000005839 Tebuconazole Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 241000238631 Hexapoda Species 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013402 health food Nutrition 0.000 description 2
- 238000004896 high resolution mass spectrometry Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000003630 growth substance Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000012106 screening analysis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000004885 tandem mass spectrometry Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000012224 working solution Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0098—Plants or trees
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/483—Physical analysis of biological material
- G01N33/4833—Physical analysis of biological material of solid biological material, e.g. tissue samples, cell cultures
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8872—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample impurities
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- General Health & Medical Sciences (AREA)
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- Immunology (AREA)
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- Optics & Photonics (AREA)
- Urology & Nephrology (AREA)
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Abstract
The invention belongs to the technical field of analysis and detection of pesticide residues in traditional Chinese medicines, and provides a method for detecting various pesticide residues in pseudo-ginseng. The pretreatment process is simple, convenient, rapid, efficient and accurate, and can be used for rapidly screening various pesticide residues and metabolites thereof in the panax notoginseng. The method adopts QuEChER dispersed solid phase extraction for sample pretreatment, has simple operation and high pesticide extraction rate; and then, according to the information such as pesticide retention time, the accurate mass number of the parent ions, the accurate mass number of the daughter ions, the secondary fragment ions and the like in a pre-established high-resolution mass spectrum database, the rapid qualitative screening quantitative determination of the pesticide residues is realized. The detection method provided by the invention can realize quality safety analysis of the pseudo-ginseng in a short time; meanwhile, the method has the characteristics of high recovery rate, strong applicability, short time consumption and high precision, each technical index can meet the requirement of daily detection and analysis of the panax notoginseng sample, and technical support is provided for ensuring the quality safety of the traditional Chinese medicine.
Description
Technical Field
The invention relates to the technical field of analysis and detection of pesticide residues in traditional Chinese medicines, in particular to a method for detecting various pesticide residues in pseudo-ginseng.
Background
Pseudo-ginseng (Panaxnotogeng) is a traditional rare Chinese medicinal material in China, is also a health food, and has the effects of promoting blood circulation to remove blood stasis, resisting inflammation, resisting tumors, resisting thrombus, reducing blood fat, enhancing immunity and the like. The pseudo-ginseng is extremely easy to be invaded by various diseases and insects in the growing process, so that pesticides are inevitably used in the planting process, and pesticide farmers excessively use the pesticides to prevent and control diseases and insect pests of the pseudo-ginseng, so that pesticide residues in the pseudo-ginseng exceed the standard and threaten human health.
Pseudo-ginseng is used as an important medicinal plant resource and a health food, and pesticide residue in the pseudo-ginseng is one of the main problems influencing the safety of the pseudo-ginseng. Therefore, both the grower and the consumer of the pseudo-ginseng and the quality safety inspection department hope to have an efficient and comprehensive inspection method for supervising and controlling the pesticide residue in the pseudo-ginseng.
The pesticides used in the planting process of panax notoginseng mainly comprise insecticides, bactericides, herbicides, growth regulators and the like, and can be classified into organic chlorine, organic phosphorus, pyrethroid vinegar, carbamate and the like according to chemical structures. The method for detecting pesticide residues in pseudo-ginseng mainly adopts gas chromatography, gas chromatography-tandem mass spectrometry, liquid chromatography and liquid chromatography-tandem mass spectrometry. Most of the detection methods aim at the detection of the same type of pesticide, and with the increase of pesticide types, the development of a detection method for simultaneously screening multiple types of pesticide residues with high flux, rapidness and efficiency is urgently needed.
Disclosure of Invention
In view of this, the present invention provides a method for detecting various pesticide residues in panax notoginseng. The detection method provided by the invention can realize high-flux and rapid detection of pesticide residues in pseudo-ginseng.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for detecting various pesticide residues in pseudo-ginseng, which comprises the following steps:
mixing the pseudo-ginseng to be detected with an extraction aid, and carrying out extraction aid to obtain an extraction aid solution;
mixing the auxiliary extract with acetonitrile, and extracting to obtain an extract;
adding a dehydrating agent and a salting-out agent into the extracting solution in sequence, and performing salting-out and centrifugation in sequence to obtain a supernatant;
mixing the supernatant with a purifying agent, and sequentially purifying and centrifuging to obtain an upper computer sample solution;
performing ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry on the upper computer sample solution to obtain chromatographic information and mass spectrometry information of the pseudo-ginseng to be detected;
searching and comparing the chromatographic information and the mass spectrum information of the pseudo-ginseng to be detected with a pre-established high-resolution mass spectrum database, determining residual pesticide components in the pseudo-ginseng to be detected, and carrying out quantitative analysis;
the ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry comprises ultra-high performance liquid chromatography detection and quadrupole/electrostatic field orbital hydrazine mass spectrometry detection;
the parameters of the ultra-high performance liquid chromatography detection comprise:
the chromatographic column is Thermo Accucore aQ, the size is 150 multiplied by 2.1mm, and the size is 2.6 mu m;
the mobile phase system comprises an aqueous phase mobile phase A and an organic phase mobile phase B;
the aqueous phase mobile phase A is an ammonium formate-formic acid aqueous solution, the concentration of ammonium formate in the ammonium formate-formic acid aqueous solution is 5mmol/L, and the volume concentration of formic acid is 0.1%;
the organic phase mobile phase B is an ammonium formate-formic acid methanol solution, the concentration of ammonium formate in the ammonium formate-formic acid methanol solution is 5mmol/L, and the volume concentration of formic acid is 0.1%;
the elution mode is gradient elution;
the procedure for the gradient elution is shown in table 1:
TABLE 1 procedure for gradient elution
| Time (min) | Volume fraction of mobile phase A (%) | Volume fraction of Mobile phase B (%) |
| 0 | 100 | 0 |
| 4 | 80 | 20 |
| 5.5 | 60 | 40 |
| 10.5 | 0 | 100 |
| 12.9 | 0 | 100 |
| 15 | 100 | 0 |
| 20 | 100 | 0 |
The parameters of the mass spectrometric detection of the quadrupole rod/electrostatic field orbitron are shown in table 2:
TABLE 2 parameters of quadrupole/Electrostatic field orbital hydrazine mass spectrometry
The pre-established high-resolution mass spectrum database comprises CAS numbers, english names, molecular formulas, chromatographic retention time, mother ion accurate mass numbers, child ion accurate mass numbers, secondary ion fragment information and linear equations of 66 pesticides;
<xnotran> 66 , , , , , , , , , , , , , , , , , , , , , , , I, , , , , , , , , , , , 3-OH , , , , , , , , , , , , , , , , , , , , , , , , , , , , , . </xnotran>
Preferably, the extraction aid comprises a glacial acetic acid solution, and the volume concentration of the glacial acetic acid solution is 1%;
the dosage ratio of the pseudo-ginseng to be detected to the extraction aid is 3g:15mL.
Preferably, the boosting mode is vortex; the rotation speed of the vortex is 1000-3500 rpm, and the time is 2-5 min;
after the lifting assistance, the patient is placed for 30min.
Preferably, the dosage ratio of the pseudo-ginseng to be detected and the acetonitrile is 3g:15mL;
the extraction mode is oscillation; the oscillation time is 5-15 min.
Preferably, the dehydrating agent includes anhydrous magnesium sulfate, and the salting-out agent includes sodium chloride; the mass ratio of the pseudo-ginseng to be detected, the dehydrating agent and the salting-out agent is 3:4:1;
the salting-out mode is oscillation; the oscillating speed is 4200-9000 rpm, and the time is 5-10 min.
Preferably, the scavenger comprises PSA, C 18 Anhydrous MgSO (MgSO) 4 And GCB; the PSA, C 18 Anhydrous MgSO (MgSO) 4 And GCB in a mass ratio of 10:10:30:3;
the dosage ratio of the supernatant to the purifying agent is 10mL:1.59g.
Preferably, the purification mode is oscillation, and the oscillation time is 5-10 min.
Preferably, the parameters of the ultra-high performance liquid chromatography detection further include: the column temperature was 30 ℃ and the flow rate of the mobile phase system was 0.3mL/min.
Preferably, the search alignment is performed on Trace Finder software.
Preferably, the quantitative analysis is performed on Trace Finder software.
The invention provides a method for detecting various pesticide residues in pseudo-ginseng, which comprises the following steps: mixing the pseudo-ginseng to be detected with an extraction aid, and carrying out extraction aid to obtain an extraction aid solution; mixing the auxiliary extract with acetonitrile, and extracting to obtain an extract; adding a dehydrating agent and a salting-out agent into the extracting solution in sequence, and performing salting-out and centrifugation in sequence to obtain a supernatant; mixing the supernatant with a purifying agent, and sequentially purifying and centrifuging to obtain an upper computer sample solution; performing ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry on the upper computer sample solution to obtain chromatographic information and mass spectrometry information of the pseudo-ginseng to be detected; searching and comparing the chromatographic information and the mass spectrum information of the pseudo-ginseng to be detected with a pre-established high-resolution mass spectrum database, determining residual pesticide components in the pseudo-ginseng to be detected, and carrying out quantitative analysis; the ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry comprises ultra-high performance liquid chromatography detection and quadrupole/electrostatic field orbital hydrazine mass spectrometry detection; the parameters of the ultra-high performance liquid chromatography detection comprise: the chromatographic column is Thermo Accucore aQ, the size is 150 multiplied by 2.1mm, and the size is 2.6 mu m; the mobile phase system comprises an aqueous phase mobile phase A and an organic phase mobile phase B; the aqueous phase mobile phase A is an ammonium formate-formic acid aqueous solution, the concentration of ammonium formate in the ammonium formate-formic acid aqueous solution is 5mmol/L, and the volume concentration of formic acid is 0.1%; the organic phase mobile phase B is an ammonium formate-formic acid methanol solution, the concentration of ammonium formate in the ammonium formate-formic acid methanol solution is 5mmol/L, and the volume concentration of formic acid is 0.1%; the elution mode is gradient elution; the procedure for the gradient elution is shown in table 1: the parameters of the mass spectrometric detection of the quadrupole rod/electrostatic field orbitron are shown in table 2: the pre-established high-resolution mass spectrum database comprises CAS numbers, english names, molecular formulas, chromatographic retention time, mother ion accurate mass numbers, child ion accurate mass numbers, secondary ion fragment information and linear equations of 66 pesticides; <xnotran> 66 , , , , , , , , , , , , , , , , , , , , , , , I, , , , , , , , , , , , 3-OH , , , , , , , , , , , , , , , , , , , , , , , , , , , , , . </xnotran>
The pretreatment process is simple, convenient, rapid, efficient and accurate, and can be used for rapidly screening various pesticide residues and metabolites in the panax notoginseng. The method adopts QuEChER dispersed solid phase extraction for sample pretreatment, has simple operation and high pesticide extraction rate; and then, according to the information such as pesticide retention time, the accurate mass number of the parent ions, the accurate mass number of the daughter ions, the secondary fragment ions and the like in a pre-established high-resolution mass spectrum database, the rapid qualitative screening quantitative determination of the pesticide residues is realized. The detection method provided by the invention can realize quality safety analysis of the pseudo-ginseng in a short time; meanwhile, the method has the characteristics of high recovery rate, strong applicability, short time consumption and high precision, each technical index can meet the requirement of daily detection and analysis of the panax notoginseng sample, and technical support is provided for guaranteeing the quality safety of the traditional Chinese medicine.
Detailed Description
The invention provides a method for detecting various pesticide residues in pseudo-ginseng, which comprises the following steps:
mixing the pseudo-ginseng to be detected with an extraction aid, and carrying out extraction aid to obtain an extraction aid solution;
mixing the auxiliary extract with acetonitrile, and extracting to obtain an extract;
adding a dehydrating agent and a salting-out agent into the extracting solution in sequence, and performing salting-out and centrifugation in sequence to obtain a supernatant;
mixing the supernatant with a purifying agent, and sequentially purifying and centrifuging to obtain an upper computer sample solution;
performing ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry on the upper computer sample solution to obtain chromatographic information and mass spectrometry information of the pseudo-ginseng to be detected;
and searching and comparing the chromatographic information and the mass spectrum information of the pseudo-ginseng to be detected with a pre-established high-resolution mass spectrum database, determining the residual pesticide components in the pseudo-ginseng to be detected, and carrying out quantitative analysis.
In the present invention, the starting materials used in the present invention are preferably commercially available products unless otherwise specified.
According to the invention, pseudo-ginseng to be detected and an extraction aid are mixed for extraction assistance to obtain an extraction aid solution.
In the invention, the pseudo-ginseng to be detected is preferably powdered pseudo-ginseng; the powder notoginseng is preferably the powder notoginseng passing through a No. 3 sieve (50 meshes).
In the present invention, the extraction aid preferably comprises a glacial acetic acid solution, and the volume concentration of the glacial acetic acid solution is preferably 1%.
In the invention, the dosage ratio of the pseudo-ginseng to be detected and the extraction aid is preferably 3g:15mL.
In the present invention, the boosting means is preferably a vortex; the rotation speed of the vortex is preferably 1000-3500 rpm, and the time is preferably 2-5 min.
After the lifting aid, the invention preferably also comprises standing for 30min.
In the invention, the extraction aid can increase the affinity between the pseudo-ginseng sample and the extractant acetonitrile, and because the plant medicine is a low-moisture sample, the interaction between the pesticide and the matrix can be weakened by adding water, and the extraction rate is improved.
After the auxiliary extract is obtained, the auxiliary extract is mixed with acetonitrile for extraction to obtain the extract.
In the invention, the dosage ratio of the pseudo-ginseng to be detected and the acetonitrile is preferably 3g:15mL.
In the present invention, the manner of extraction is preferably shaking; the time of the oscillation is preferably 5 to 15min.
After the extracting solution is obtained, the dehydrating agent and the salting-out agent are sequentially added into the extracting solution, and salting-out and centrifugation are sequentially carried out to obtain a supernatant.
In the present invention, the dehydrating agent preferably includes anhydrous magnesium sulfate. In the present invention, the salting-out agent preferably includes sodium chloride. In the invention, the mass ratio of the pseudo-ginseng to be measured, the dehydrating agent and the salting-out agent is preferably 3:4:1.
in the present invention, the salting-out is preferably performed by shaking; the rotating speed of the oscillation is preferably 4200-9000 rpm; the time of the oscillation is preferably 5 to 10min.
The parameters of the centrifugation are not particularly limited in the present invention as long as the separation of solid and liquid can be achieved.
In the invention, acetonitrile has high extraction efficiency of pesticides, particularly polar pesticides, has good purification effect of the adsorbent, and less extraction of nonpolar ingredients such as starch, pigment, wax and the like in the matrix, and water is easier to remove by salting out.
After the supernatant is obtained, the supernatant and the purifying agent are mixed, and purification and centrifugation are sequentially carried out to obtain the upper computer sample solution.
In the present invention, the scavenger preferably comprises PSA, C 18 Anhydrous MgSO (MgSO) in water 4 And GCB; the PSA, C 18 Anhydrous MgSO (MgSO) 4 And GCB are preferably in a mass ratio of 10:10:30:3.
in the present invention, the amount ratio of the supernatant to the depurative is preferably 10mL:1.59g.
In the invention, the purification mode is preferably oscillation, and the oscillation time is preferably 5-10 min.
The present invention does not specifically limit the manner of centrifugation, as long as solids and liquids can be separated.
After the upper computer sample solution is obtained, the invention carries out ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry on the upper computer sample solution to obtain the chromatographic information and the mass spectrometry information of the pseudo-ginseng to be detected.
In the invention, the ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry comprises ultra-high performance liquid chromatography detection and quadrupole/electrostatic field orbital hydrazine mass spectrometry detection;
the parameters of the ultra-high performance liquid chromatography detection comprise:
the chromatographic column is Thermo Accucore aQ, the size is 150 multiplied by 2.1mm, and the size is 2.6 mu m;
the mobile phase system comprises an aqueous phase mobile phase A and an organic phase mobile phase B;
the aqueous phase mobile phase A is an ammonium formate-formic acid aqueous solution, the concentration of ammonium formate in the ammonium formate-formic acid aqueous solution is 5mmol/L, and the volume concentration of formic acid is 0.1%;
the organic phase mobile phase B is an ammonium formate-formic acid methanol solution, the concentration of ammonium formate in the ammonium formate-formic acid methanol solution is 5mmol/L, and the volume concentration of formic acid is 0.1%;
the elution mode is gradient elution;
the procedure for the gradient elution is shown in table 1.
In the invention, the parameters of the ultra high performance liquid chromatography detection further include: the column temperature is preferably 30 ℃ and the flow rate of the mobile phase system is preferably 0.3mL/min.
In the invention, the parameters of the quadrupole/electrostatic field orbital hydrazine mass spectrometry are shown in table 2.
In the invention, the chromatographic information of the pseudo-ginseng to be detected preferably comprises retention time, chromatographic peak area, chromatographic peak height and a linear equation; the mass spectrum information of the pseudo-ginseng to be detected preferably comprises a parent ion accurate mass number, a child ion accurate mass number and a secondary fragment ion.
After the chromatographic information and the mass spectrum information of the pseudo-ginseng to be detected are obtained, the chromatographic information and the mass spectrum information of the pseudo-ginseng to be detected are searched and compared with a pre-established high-resolution mass spectrum database, the residual pesticide components in the pseudo-ginseng to be detected are determined, and quantitative analysis is carried out.
In the invention, the pre-established high-resolution mass spectrum database comprises CAS numbers, english names, molecular formulas, chromatographic retention time, accurate mass numbers of parent ions, accurate mass numbers of child ions, secondary ion fragment information and linear equations of 66 pesticides.
<xnotran> , 66 , , , , , , , , , , , , , , , , , , , , , , , I, , , , , , , , , , , , 3-OH , , , , , , , , , , , , , , , , , , , , , , , , , , , , , . </xnotran>
In the present invention, the pre-established high resolution mass spectra database is shown in table 3.
TABLE 3 Pre-built high resolution mass spectra database
In the present invention, the acquisition mode of the chromatographic retention time, the precise mass number of parent ions, the precise mass number of daughter ions, and the secondary ion fragment information of the 66 pesticides in the pre-established high resolution mass spectrum database preferably includes the following steps:
metering the volume of 66 pesticide standard substances with methanol to prepare a standard stock solution; diluting the standard stock solution into a standard intermediate solution by using methanol;
and carrying out ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry on the standard intermediate solution to obtain the chromatographic retention time, the accurate mass number of parent ions, the accurate mass number of daughter ions and the information of secondary ion fragments of 66 pesticide standard samples.
In the present invention, the concentration of the 66 pesticide standards in the standard stock solution is independently preferably 50mg/L. In the present invention, the concentration of the 66 pesticides in the standard intermediate solution is independently preferably 1 to 10mg/L.
In the invention, the parameters of the ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry detection are preferably consistent with the technical scheme, and are not described herein again.
In the present invention, the CAS number, english name and molecular formula of the 66 pesticides in the pre-established high resolution mass spectrum database are preferably obtained by query.
In the present invention, the linear equations of the 66 pesticides in the pre-established high resolution mass spectrum database are preferably established by a linear equation establishment method well known to those skilled in the art.
In the present invention, the search alignment is preferably performed on TraceFinder software.
In the present invention, the search alignment principle preferably includes: deviation between chromatographic peak retention time of pseudo-ginseng to be detected and retention time in a pre-established high-resolution mass spectrum database is within +/-2.5%, deviation between a precise mass number of parent ions and a theoretical mass number is less than or equal to 5ppm, deviation between at least 2 fragment ions with high abundance in secondary fragment ions and corresponding fragment ions in the spectrum database is less than or equal to 5ppm, and abundance of the secondary fragment ions is consistent with that of corresponding fragment ions in standard working solution with approximate concentration, so that the pseudo-ginseng to be detected can be judged to contain the pesticide.
In the present invention, the quantitative analysis is preferably performed on the TraceFinder software.
In the present invention, the quantitative analysis is preferably performed on the target by using an external standard method using parent ions as the quantitative ions.
The following examples are provided to describe the method for detecting various pesticide residues in panax notoginseng according to the present invention in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Creation of pre-built high resolution mass spectrometry database
Preparing a pesticide standard solution: the pesticide standard substance is fixed in volume by methanol, and is prepared into standard stock solution with the concentration of each standard substance being 50 mg/L; diluting the standard stock solution into a standard intermediate solution with the concentration of each pesticide standard substance of 10mg/L by using methanol; the 66 kinds of pesticides are as follows: <xnotran> , , , , , , , , , , , , , , , , , , , , , , , I, , , , , , , , , , , , 3-OH , , , , , , , , , , , , , , , , , , , , , , , , , , , , , . </xnotran>
Performing ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry on the obtained standard solution to obtain the chromatographic retention time, the accurate mass number of the parent ions, the accurate mass number of the daughter ions and the information of the secondary ion fragments of the standard solution, which are specifically shown in table 3.
The ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry detection comprises ultra-high performance liquid chromatography detection and quadrupole/electrostatic field orbital hydrazine mass spectrometry detection;
wherein, the parameters of the ultra-high performance liquid chromatography detection comprise: the chromatographic column is Thermo Accucore aQ, the size is 150 multiplied by 2.1mm, and the size is 2.6 mu m; the column temperature is 30 ℃; the mobile phase system comprises an aqueous phase mobile phase A and an organic phase mobile phase B; the flow rate of the mobile phase system is 0.3mL/min; the aqueous phase mobile phase A is an ammonium formate-formic acid aqueous solution, the concentration of ammonium formate in the ammonium formate-formic acid aqueous solution is 5mmol/L, and the volume concentration of formic acid is 0.1%; the organic phase mobile phase B is an ammonium formate-formic acid methanol solution, the concentration of ammonium formate in the ammonium formate-formic acid methanol solution is 5mmol/L, and the volume concentration of formic acid is 0.1%; the elution mode is gradient elution; the procedure for gradient elution is shown in table 1.
The parameters of mass spectrometric detection of quadrupole/electrostatic field orbitron are shown in table 2.
The mixed standard solution of 66 pesticides is prepared into standard curves of 5 mug/L, 25 mug/L, 50 mug/L, 100 mug/L, 250 mug/L and 500 mug/L respectively by adopting blank matrix solution. And (3) carrying out chromatographic mass spectrometry detection on the standard curves with different concentrations, and establishing a linear equation according to the chromatographic peak area (y) of the full-scanning parent ion and the concentration (x, mu g/L) of the analyte for quantification when the sample size is 5 mu L, wherein the obtained linear equation is shown in table 3. As can be seen from table 3: the correlation coefficient (r) was greater than 0.99 for all compounds, indicating good linearity. The CAS number, english name and molecular formula of the 66 pesticides are preferably obtained by query and are reported in table 3.
Example 2
In order to verify the accuracy and precision of the detection method, 66 pesticide residue mixed standards with mass concentrations of 10, 50 and 100 mu g/L are respectively added into a blank pseudo-ginseng sample, ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry detection is carried out according to a pretreatment method and the same instrument conditions, and each level is repeated for 6 times. The precision of the method was investigated in terms of the relative standard deviation of the measurements and the spiked recovery was calculated for different concentrations, and the results are detailed in table 4.
The pretreatment method comprises the following steps: 3g of pseudo-ginseng sample powder (sieved by a third sieve), precisely weighing, and addingCollecting 1% glacial acetic acid solution 15mL, vortex standing for 30min, adding acetonitrile 15mL precisely, shaking for 5min, adding anhydrous MgSO 4g 4 And 1g NaCl, evenly mixed by vortex, centrifuged, and 10mL of supernatant is taken and added with purifying agent (300mgPSA +300mgC18+900mg anhydrous MgSO 4 +90 mgGCB) and filtering to obtain the sample.
3. And (3) detecting by using a chromatographic mass spectrum: and analyzing the sample by using an ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry combined analysis method. Conditions of ultra-high performance liquid chromatography detection: and (3) chromatographic column: thermo AccucoreaQ (150 × 2.1mm,2.6 μm), column temperature: 30 ℃, flow rate: 0.3mL/min, positive ion FullMS-ddMS 2 Scanning mode: mobile phase a is aqueous phase: 5mmol/L ammonium formate and 0.1% aqueous formic acid; the mobile phase B is an organic phase: 5mmol/L ammonium formate and 0.1% methanolic formic acid 0.1% aqueous formic acid.
The parameters of ultra performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry detection are the same as in example 1.
Repeatability and recovery rate results of 466 pesticide residue methods
As can be seen from Table 4, the recovery rate is 70-120%, and the Relative Standard Deviation (RSD) is less than 10%, which shows that the method has good accuracy and high precision, and can be used for detecting and analyzing various pesticide residues in the pseudo-ginseng.
Example 3
The practicability of the detection method provided by the invention in actual sample detection is further evaluated by detecting a commercially available pseudo-ginseng sample. The detection method of the present invention was applied to 50 specimens from a retail pharmacy for non-targeted screening analysis and the presence of pesticide residues was quantified by using the matrix matching calibration curve of the present invention.
Precisely weighing 3g of Notoginseng radix powder to be tested (sieved with a third sieve), adding 1% glacial acetic acid solution 15mL, vortex standing for 30min, precisely adding acetonitrile 15mL, shaking for 5min, adding 4g anhydrous MgSO 4 And 1g NaCl, evenly mixed by vortex, centrifuged, and 10mL of supernate is taken and added with a purifying agent (300mg PSA +300mg C) 18 +900mg of anhydrous MgSO 4 +90mg GCB) is vortexed, mixed and shaken for 5min, and centrifuged and filtered to obtain an upper computer sample.
Detecting the upper computer sample according to the parameters of the ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry detection in the embodiment 1 to obtain the chromatographic information and the high-resolution mass spectrometry information of the pseudo-ginseng sample to be detected.
And searching and comparing the obtained chromatographic information and mass spectrum information of the pseudo-ginseng sample with a database in a table 3, and determining that the tested pseudo-ginseng sample contains pesticides dimethomorph, oxadixyl, tebuconazole, thiophanate-methyl and difenoconazole.
Quantitative analysis is carried out on dimethomorph, oxadixyl, tebuconazole, thiophanate-methyl and difenoconazole in the pseudo-ginseng powder to be detected by using a matrix matching calibration curve in a table 3, and the obtained results show that the content of dimethomorph, oxadixyl, thiophanate-methyl and difenoconazole in the pseudo-ginseng sample to be detected is 0.058-2.45 mg/kg, the content of oxadixyl is 0.045-1.38 mg/kg, the content of tebuconazole is 0.44-2.30 mg/kg, the content of thiophanate-methyl is 0.072-0.86 mg/kg and the content of difenoconazole is 0.065-5.40 mg/kg.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for detecting various pesticide residues in pseudo-ginseng is characterized by comprising the following steps:
mixing the pseudo-ginseng to be detected with an extraction aid, and carrying out extraction aid to obtain an extraction aid solution;
mixing the auxiliary extract with acetonitrile, and extracting to obtain an extract;
adding a dehydrating agent and a salting-out agent into the extracting solution in sequence, and performing salting-out and centrifugation in sequence to obtain a supernatant;
mixing the supernatant with a purifying agent, and sequentially purifying and centrifuging to obtain an upper computer sample solution;
performing ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry on the upper computer sample solution to obtain chromatographic information and mass spectrometry information of the pseudo-ginseng to be detected;
searching and comparing the chromatographic information and the mass spectrum information of the pseudo-ginseng to be detected with a pre-established high-resolution mass spectrum database, determining the residual pesticide components in the pseudo-ginseng to be detected, and carrying out quantitative analysis;
the ultra-high performance liquid chromatography-quadrupole/electrostatic field orbital hydrazine mass spectrometry comprises ultra-high performance liquid chromatography detection and quadrupole/electrostatic field orbital hydrazine mass spectrometry detection;
the parameters of the ultra-high performance liquid chromatography detection comprise:
the chromatographic column is ThermoAccucore aQ, the size is 150 multiplied by 2.1mm, and the size is 2.6 mu m;
the mobile phase system comprises an aqueous phase mobile phase A and an organic phase mobile phase B;
the aqueous phase mobile phase A is an ammonium formate-formic acid aqueous solution, the concentration of ammonium formate in the ammonium formate-formic acid aqueous solution is 5mmol/L, and the volume concentration of formic acid is 0.1%;
the organic phase mobile phase B is an ammonium formate-formic acid methanol solution, the concentration of ammonium formate in the ammonium formate-formic acid methanol solution is 5mmol/L, and the volume concentration of formic acid is 0.1%;
the elution mode is gradient elution;
the procedure for the gradient elution is shown in table 1:
TABLE 1 procedure for gradient elution
The parameters of the mass spectrometric detection of the quadrupole rod/electrostatic field orbitron are shown in table 2:
TABLE 2 parameters of quadrupole/Electrostatic field orbital hydrazine mass spectrometry
The pre-established high-resolution mass spectrum database comprises CAS numbers, english names, molecular formulas, chromatographic retention time, accurate parent ion mass numbers, accurate child ion mass numbers, secondary ion fragment information and linear equations of 66 pesticides;
<xnotran> 66 , , , , , , , , , , , , , , , , , , , , , , , I, , , , , , , , , , , , 3-OH , , , , , , , , , , , , , , , , , , , , , , , , , , , , , . </xnotran>
2. The detection method according to claim 1, wherein the extraction aid comprises a glacial acetic acid solution, and the volume concentration of the glacial acetic acid solution is 1%;
the dosage ratio of the pseudo-ginseng to be detected to the extraction aid is 3g:15mL.
3. The detection method according to claim 1 or 2, wherein the boosting mode is vortexing; the rotation speed of the vortex is 1000-3500 rpm, and the time is 2-5 min;
after the lifting assistance, the standing is also included for 30min.
4. The detection method according to claim 1, wherein the dosage ratio of the pseudo-ginseng to be detected to the acetonitrile is 3g:15mL;
the extraction mode is oscillation; the oscillation time is 5-15 min.
5. The detection method according to claim 1, wherein the dehydrating agent comprises anhydrous magnesium sulfate, and the salting-out agent comprises sodium chloride; the mass ratio of the pseudo-ginseng to be detected, the dehydrating agent and the salting-out agent is 3:4:1;
the salting-out mode is oscillation; the oscillating speed is 4200-9000 rpm, and the time is 5-10 min.
6. The detection method according to claim 1, wherein the scavenger comprises PSA, C 18 Anhydrous MgSO (MgSO) 4 And GCB; the PSA, C 18 Anhydrous MgSO (MgSO) in water 4 And GCB in a mass ratio of 10:10:30:3;
the dosage ratio of the supernatant to the purifying agent is 10mL:1.59g.
7. The detection method according to claim 1 or 6, wherein the purification is performed by shaking, and the shaking time is 5-10 min.
8. The detection method according to claim 1, wherein the parameters of the ultra performance liquid chromatography detection further comprise: the column temperature was 30 ℃ and the flow rate of the mobile phase system was 0.3mL/min.
9. The detection method according to claim 1, wherein the search alignment is performed on Trace Finder software.
10. The assay of claim 1 wherein the quantitative analysis is performed on Trace Finder software.
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| CN102735784B (en) * | 2011-04-11 | 2014-11-12 | 中国科学院长春应用化学研究所 | Method for simultaneously determining one hundred pesticide residuals in traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum |
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