CN112730678A - Method for simultaneously detecting and analyzing various pesticide residues in fruits and vegetables - Google Patents
Method for simultaneously detecting and analyzing various pesticide residues in fruits and vegetables Download PDFInfo
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- CN112730678A CN112730678A CN202011548939.3A CN202011548939A CN112730678A CN 112730678 A CN112730678 A CN 112730678A CN 202011548939 A CN202011548939 A CN 202011548939A CN 112730678 A CN112730678 A CN 112730678A
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- 235000012055 fruits and vegetables Nutrition 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000000447 pesticide residue Substances 0.000 title claims abstract description 14
- 101710117064 Trimethylamine corrinoid protein 1 Proteins 0.000 claims abstract description 13
- DUEPRVBVGDRKAG-UHFFFAOYSA-N carbofuran Chemical compound CNC(=O)OC1=CC=CC2=C1OC(C)(C)C2 DUEPRVBVGDRKAG-UHFFFAOYSA-N 0.000 claims abstract description 13
- SBPBAQFWLVIOKP-UHFFFAOYSA-N chlorpyrifos Chemical compound CCOP(=S)(OCC)OC1=NC(Cl)=C(Cl)C=C1Cl SBPBAQFWLVIOKP-UHFFFAOYSA-N 0.000 claims abstract description 13
- OEBRKCOSUFCWJD-UHFFFAOYSA-N dichlorvos Chemical compound COP(=O)(OC)OC=C(Cl)Cl OEBRKCOSUFCWJD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229950001327 dichlorvos Drugs 0.000 claims abstract description 13
- NFACJZMKEDPNKN-UHFFFAOYSA-N trichlorfon Chemical compound COP(=O)(OC)C(O)C(Cl)(Cl)Cl NFACJZMKEDPNKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- RHSUJRQZTQNSLL-UHFFFAOYSA-N 3-Hydroxy-carbofuran Chemical compound CNC(=O)OC1=CC=CC2=C1OC(C)(C)C2O RHSUJRQZTQNSLL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000005944 Chlorpyrifos Substances 0.000 claims abstract description 10
- JLQUFIHWVLZVTJ-UHFFFAOYSA-N carbosulfan Chemical compound CCCCN(CCCC)SN(C)C(=O)OC1=CC=CC2=C1OC(C)(C)C2 JLQUFIHWVLZVTJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003814 drug Substances 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000575 pesticide Substances 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- 239000002207 metabolite Substances 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 230000010355 oscillation Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 229940079593 drug Drugs 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001819 mass spectrum Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000012086 standard solution Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- FATBKZJZAHWCSL-UHFFFAOYSA-N 2,3,5,6-tetrachloropyridine Chemical compound ClC1=CC(Cl)=C(Cl)N=C1Cl FATBKZJZAHWCSL-UHFFFAOYSA-N 0.000 claims description 3
- -1 O, O-dimethyl- (2,2, 2-trichloro-1-hydroxyethyl) phosphonate ester Chemical class 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000007857 degradation product Substances 0.000 claims description 3
- 239000000543 intermediate Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000003986 organophosphate insecticide Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 10
- 238000004458 analytical method Methods 0.000 abstract description 6
- 238000012216 screening Methods 0.000 abstract description 4
- 229960001952 metrifonate Drugs 0.000 abstract description 3
- 238000004949 mass spectrometry Methods 0.000 abstract description 2
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 241000220225 Malus Species 0.000 description 2
- 235000021016 apples Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WYEMLYFITZORAB-UHFFFAOYSA-N boscalid Chemical compound C1=CC(Cl)=CC=C1C1=CC=CC=C1NC(=O)C1=CC=CN=C1Cl WYEMLYFITZORAB-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- HQVFCQRVQFYGRJ-UHFFFAOYSA-N formic acid;hydrate Chemical compound O.OC=O HQVFCQRVQFYGRJ-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 1
- 238000012502 risk assessment Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a method for simultaneously detecting and analyzing various pesticide residues in fruits and vegetables, which comprises the following specific steps: the method comprises the steps of preparing a medicine to be detected, pretreating a detection sample, processing the detection sample, analyzing and determining trichlorfon, carbofuran, dichlorvos, TCP-1, chlorpyrifos, carbosulfan and 3-hydroxy carbofuran in fruits and vegetables by adopting HPLCMSMS (liquid chromatography tandem mass spectrometry), screening a proper detection and analysis method, namely the method, and establishing an optimal method. And (3) determining a detection method and verifying a result by screening parameters such as chromatographic columns, mobile phases, chromatographic mass spectrometry conditions and the like.
Description
Technical Field
The invention relates to the field of fruit and vegetable pesticide residue detection, in particular to a method for simultaneously detecting and analyzing various pesticide residues in fruits and vegetables.
Background
The detection of pesticide residues in agricultural products is an important link for guaranteeing the quality and safety of the agricultural products. Many pesticides are easy to decompose and degrade into metabolites of isomers thereof, and if the pesticides and the metabolites thereof cannot be analyzed together, medication conditions of products can be missed and misjudged, and pesticide risk conditions in agricultural products cannot be well evaluated. The existing pesticide residues on fruits and vegetables mainly comprise dipterex, carbofuran, dichlorvos, TCP-1, chlorpyrifos, carbosulfan, 3-hydroxy carbofuran and the like, and the existing pesticide residues on the fruits and vegetables need to be detected and compared one by one respectively to detect whether the fruits and vegetables have the pesticide residues, so that a great deal of waste of manpower, material resources and time is caused by independent analysis.
Disclosure of Invention
According to the technical problems, the invention provides a method for simultaneously detecting and analyzing various pesticide residues in fruits and vegetables, which comprises the following specific steps:
firstly, preparing the drugs to be detected as dipterex, carbofuran, dichlorvos, TCP-1, chlorpyrifos, carbosulfan and 3-hydroxy carbofuran, wherein the dichlorvos are degradation products of the dipterex, the carbofuran and the 3-hydroxy carbofuran are metabolites of the carbofuran, the TCP-1 and the TCP are pesticide metabolites of the chlorpyrifos, the chemical name of the dipterex is O, O-dimethyl- (2,2, 2-trichloro-1-hydroxyethyl) phosphonate ester, an organophosphorus insecticide, an industrial product is a white solid, the melting point of a pure product is 83-84 ℃, the pure product can be dissolved in water and an organic solvent, the property is stable, but the pure product is hydrolyzed into the dichlorvos when being subjected to alkali; TCP and TCP-1 are chemically named as 2,3,5, 6-tetrachloropyridine, are pesticide intermediates and are chlorpyrifos metabolites;
cleaning the fruits and vegetables to be detected, then smashing the fruit and vegetable samples, then homogenizing, weighing 10g of the homogenized samples in a 50mL centrifugal device;
adding 10mL of acetonitrile into the centrifugal device, covering a centrifugal cover, and carrying out vortex oscillation for 1 min;
opening the centrifugal device, adding QuECHERS pretreatment extraction salt packets and 1 ceramic homogeneous proton, covering a centrifugal cover, and carrying out vortex oscillation for 1 min;
fifthly, after shaking, centrifuging for 5min at a speed of 4200 r/min;
sixthly, sucking 6mL of supernatant, adding the supernatant into a 15mL purification tube for QuECHERS pretreatment, and centrifuging for 5min at 4200 r/min;
seventhly, taking and sucking 2mL of supernate into a 10mL test tube, and blowing nitrogen to be nearly dry in a water bath at 40 ℃;
eighthly, adding 20 mu L of internal standard solution, adding 1mL of ethyl acetate for redissolution, and filtering the mixture through a microporous filter membrane;
and ninthly, measuring on a liquid chromatogram tandem mass spectrum combination instrument.
The centrifugal device is a centrifugal tube
The centrifugal device is a chromatographic column.
The use conditions of the liquid chromatogram tandem mass spectrum combination instrument are as follows:
analyzing a chromatographic column: hypersil GOLDTM (Thermo) (100 mm. times.2.1 mm,1.9 μm);
the flow rate is 0.3 mL/min;
the temperature of the chromatographic column is 40 ℃;
the sample injection volume is 10 mu L;
mobile phase and elution conditions: 0.1% formic acid water, 0-1min methanol, 10% B, 1.1-4min methanol, 55% B,4.1-6 min: 80% of B, 6.1-12min: 95% of B,12.1-14: 10% of B. The invention has the beneficial effects that: by adopting HPLCMSMS (liquid chromatography tandem mass spectrometer) to analyze and measure trichlorfon, carbofuran, dichlorvos, TCP-1, chlorpyrifos, carbosulfan and 3-hydroxy carbofuran in fruits and vegetables, screening a proper detection and analysis method, namely the method, the optimal method is established. And (3) determining a detection method and verifying a result by screening parameters such as chromatographic columns, mobile phases, chromatographic mass spectrometry conditions and the like.
The invention adopts a proper detection method to simultaneously analyze the pesticide and the metabolite thereof, and has important significance for agricultural product detection and agricultural product risk assessment. The method is intended to research the simultaneous analysis methods of trichlorfon, carbofuran, dichlorvos, TCP-1, chlorpyrifos, carbosulfan and 3-hydroxy carbofuran in fruits and vegetables, so as to seek a proper analysis method to analyze the substances together. And a great deal of waste of manpower, material resources and time caused by the independent analysis of each substance is reduced.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention is further illustrated with reference to fig. 1:
example 1
A method for simultaneously detecting and analyzing various pesticide residues in fruits and vegetables comprises the following specific test methods:
firstly, preparing the drugs to be detected as dipterex, carbofuran, dichlorvos, TCP-1, chlorpyrifos, carbosulfan and 3-hydroxy carbofuran, wherein the dichlorvos are degradation products of the dipterex, the carbofuran and the 3-hydroxy carbofuran are metabolites of the carbofuran, the TCP-1 and the TCP are pesticide metabolites of the chlorpyrifos, the chemical name of the dipterex is O, O-dimethyl- (2,2, 2-trichloro-1-hydroxyethyl) phosphonate ester, an organophosphorus insecticide, an industrial product is a white solid, the melting point of a pure product is 83-84 ℃, the pure product can be dissolved in water and an organic solvent, the property is stable, but the pure product is hydrolyzed into the dichlorvos when being subjected to alkali; TCP and TCP-1 are chemically named as 2,3,5, 6-tetrachloropyridine, are pesticide intermediates and are chlorpyrifos metabolites;
cleaning the fruits and vegetables to be detected, then smashing the fruit and vegetable samples, then homogenizing, weighing 10g of the homogenized samples in a 50mL centrifugal device;
adding 10mL of acetonitrile into the centrifugal device, covering a centrifugal cover, and carrying out vortex oscillation for 1 min;
opening the centrifugal device, adding QuECHERS pretreatment extraction salt packets and 1 ceramic homogeneous proton, covering a centrifugal cover, and carrying out vortex oscillation for 1 min;
fifthly, after shaking, centrifuging for 5min at a speed of 4200 r/min;
sixthly, sucking 6mL of supernatant, adding the supernatant into a 15mL purification tube for QuECHERS pretreatment, and centrifuging for 5min at 4200 r/min;
seventhly, taking and sucking 2mL of supernate into a 10mL test tube, and blowing nitrogen to be nearly dry in a water bath at 40 ℃;
eighthly, adding 20 mu L of internal standard solution, adding 1mL of ethyl acetate for redissolution, and filtering the mixture through a microporous filter membrane;
and ninthly, measuring on a liquid chromatogram tandem mass spectrum combination instrument.
Example 2
When the apples are detected, the apples to be detected are cleaned, cut up, homogenized, and 10g of the homogenized sample is weighed in a 50mL centrifugal device; adding 10mL of acetonitrile into a centrifugal device, covering a centrifugal cover, and carrying out vortex oscillation for 1 min; opening the centrifugal device, adding QuECHERS pretreatment extraction salt packets and 1 ceramic homogeneous proton, covering a centrifugal cover, and carrying out vortex oscillation for 1 min; after shaking, centrifuging for 5min at 4200 r/min; absorbing 6mL of supernatant, adding the supernatant into a 15mL purification tube for QuECHERS pretreatment, and centrifuging for 5min at 4200 r/min; 2mL of supernatant is taken and sucked into a 10mL test tube, and nitrogen is blown to be nearly dry in a water bath at 40 ℃; adding 20 mu L of internal standard solution, adding 1mL of ethyl acetate for redissolution, and filtering by using a microporous filter membrane; measured on a triple quadrupole tandem mass spectrometer (TSQ ENDURA, Thermo, u.s.a.) of an Electrospray (ESI) ion source, set with the following conditions:
ionization source polarity: positive and negative modes
Atomizing: nitrogen gas
Ion spray voltage: 3000V (ESI +)4326(ESI-)
Sheath gas: 60Arb
Auxiliary gas: 15Arb
Back blowing: 0Arb
Ion transfer tube temperature: 200 deg.C
Temperature of the atomizer: 400 deg.C
Collision gas and pressure: argon gas 1.5m Torr;
the scan pattern, ion pair, collision energy, RF Lens, of each component is as follows
Finally, the data are collected and processed by using Thermo TraceFinder 4.1General Quan software.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. While the invention has been described with respect to the above embodiments, it will be understood by those skilled in the art that the invention is not limited to the above embodiments, which are described in the specification and illustrated only to illustrate the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (3)
1. A method for simultaneously detecting and analyzing various pesticide residues in fruits and vegetables comprises the following specific test methods:
firstly, preparing the drugs to be detected as dipterex, carbofuran, dichlorvos, TCP-1, chlorpyrifos, carbosulfan and 3-hydroxy carbofuran, wherein the dichlorvos are degradation products of the dipterex, the carbofuran and the 3-hydroxy carbofuran are metabolites of the carbofuran, the TCP-1 and the TCP are pesticide metabolites of the chlorpyrifos, the chemical name of the dipterex is O, O-dimethyl- (2,2, 2-trichloro-1-hydroxyethyl) phosphonate ester, an organophosphorus insecticide, an industrial product is a white solid, the melting point of a pure product is 83-84 ℃, the pure product can be dissolved in water and an organic solvent, the property is stable, but the pure product is hydrolyzed into the dichlorvos when being subjected to alkali; TCP and TCP-1 are chemically named as 2,3,5, 6-tetrachloropyridine, are pesticide intermediates and are chlorpyrifos metabolites;
cleaning the fruits and vegetables to be detected, then smashing the fruit and vegetable samples, then homogenizing, weighing 10g of the homogenized samples in a 50mL centrifugal device;
adding 10mL of acetonitrile into the centrifugal device, covering a centrifugal cover, and carrying out vortex oscillation for 1 min;
opening the centrifugal device, adding QuECHERS pretreatment extraction salt packets and 1 ceramic homogeneous proton, covering a centrifugal cover, and carrying out vortex oscillation for 1 min;
fifthly, after shaking, centrifuging for 5min at a speed of 4200 r/min;
sixthly, sucking 6mL of supernatant, adding the supernatant into a 15mL purification tube for QuECHERS pretreatment, and centrifuging for 5min at 4200 r/min;
seventhly, taking and sucking 2mL of supernate into a 10mL test tube, and blowing nitrogen to be nearly dry in a water bath at 40 ℃;
eighthly, adding 20 mu L of internal standard solution, adding 1mL of ethyl acetate for redissolution, and filtering the mixture through a microporous filter membrane;
and ninthly, measuring on a liquid chromatogram tandem mass spectrum combination instrument.
2. The method for simultaneously detecting and analyzing multiple pesticide residues in fruits and vegetables according to claim 1, wherein the centrifugal device is a centrifugal tube
3. The method for simultaneously detecting and analyzing multiple pesticide residues in fruits and vegetables according to claim 1, wherein the centrifugal device is a chromatographic column.
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Citations (4)
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---|---|---|---|---|
CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
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CN111007185A (en) * | 2019-12-30 | 2020-04-14 | 广电计量检测(湖南)有限公司 | Method for determining pesticide residue in edible plant enzyme |
-
2020
- 2020-12-24 CN CN202011548939.3A patent/CN112730678A/en active Pending
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CN102221589A (en) * | 2011-03-28 | 2011-10-19 | 中国水稻研究所 | Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer |
CN107976490A (en) * | 2017-09-29 | 2018-05-01 | 沈阳出入境检验检疫局检验检疫综合技术中心 | The remaining method of pesticide in one kind detection veterinary antibiotics |
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CN111007185A (en) * | 2019-12-30 | 2020-04-14 | 广电计量检测(湖南)有限公司 | Method for determining pesticide residue in edible plant enzyme |
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