CN115219624A - Rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials - Google Patents

Rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials Download PDF

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CN115219624A
CN115219624A CN202210833282.8A CN202210833282A CN115219624A CN 115219624 A CN115219624 A CN 115219624A CN 202210833282 A CN202210833282 A CN 202210833282A CN 115219624 A CN115219624 A CN 115219624A
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chinese medicinal
sample
traditional chinese
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forbidden
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闫艳华
王帅
刘会会
王雅静
张亮
周彦成
赵海涛
谷守国
沈立茹
郑百芹
张旭
侯俊杰
单睿琪
李林
佟尧
张贺凤
李静伟
王艳玲
张金红
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Tangshan Food And Drug Comprehensive Inspection And Testing Center Tangshan Agricultural Product Quality And Safety Inspection And Testing Center Tangshan Inspection And Testing Research Institute
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • 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
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Abstract

The invention provides a rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials, and belongs to the technical field of pesticide detection. According to the invention, different extraction solvents and purification reagents are selected, so that the pretreatment purification steps are optimized, and the experiment efficiency is improved; impurities are removed, damage to a chromatographic column and a mass spectrometer is reduced, conditions of high performance liquid chromatography-tandem mass spectrometry are optimized, and accuracy and precision of detection results are improved. The method has the advantages of shortening the sample pretreatment time, having high automation degree, saving the detection time, greatly reducing the use amount and the types of organic reagents, reducing the detection cost, being environment-friendly, having high detection sensitivity and data accuracy, processing more samples at one time and greatly improving the detection efficiency.

Description

Rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials
Technical Field
The invention relates to the technical field of pesticide detection, in particular to a rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials.
Background
During the planting and production of Chinese medicinal materials, organophosphorus and carbamate pesticides are widely used, and the two pesticides both have action mechanisms of losing the ability of decomposing acetylcholine through the close combination with the active part of acetylcholinesterase. Organophosphorus and carbamate pesticides are harmful to human bodies while removing pests, so that the monitoring of pesticide residues is particularly important.
However, in the prior art, the detection index of pesticide residue in the traditional Chinese medicine is single, the pretreatment process is complex, the dosage of organic reagents is large, the environment pollution is caused, the health of technical personnel is damaged, and the time and labor are wasted.
Disclosure of Invention
In view of the above, the invention provides a rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials, which takes a pharmacopoeia detection method as a comparison, optimizes a pretreatment purification step by selecting different extraction solvents and purification reagents, and improves the experimental efficiency; the method has the advantages of removing impurities, reducing damage to the chromatographic column and the mass spectrometer, optimizing the conditions of high performance liquid chromatography-tandem mass spectrometry and improving the accuracy and precision of detection results.
The 33 forbidden pesticides in the invention are methamidophos, aldicarb sulfoxide, aldicarb sulfone, monocrotophos, chlordime, 3-hydroxy carbofuran, aldicarb, phosphamidon, thiocyclophos, fenamiphos sulfoxide, carbofuran, fenamiphos sulfone, isocarbophos, phorate sulfoxide, metsulfuron-methyl, chlorsulfuron, phorate sulfone, tribenuron-methyl, demeton-o, demeton-s, terbufos sulfoxide, terbufos sulfone, fenamiphos, isazophos, methyl isothion, sulfotep, cadusafos, disulfoton, phorum, terbufos and coumaphos.
The method for rapidly detecting the 33 forbidden pesticide residues in the traditional Chinese medicinal materials comprises the following steps:
(1) Preparing a sample solution: crushing a traditional Chinese medicine sample to be detected into powder, sieving the powder by using a 80-mesh sieve, adding the powder into a centrifugal tube, adding water, adding acetonitrile after uniformly mixing the powder by vortex, and then adding an extracting agent, zirconium beads and a purifying agent to obtain a sample solution;
(2) Pretreatment: after the sample solution obtained in the step (1) is subjected to alternate oscillation and centrifugation for 25min, purifying liquid is obtained, the purifying liquid is taken to pass through an organic microporous filter membrane with the diameter of 0.22 mu m, and the obtained filtrate is subjected to LC-MS/MS measurement;
(3) Mixing a sample blank extracting solution: taking a blank sample, and preparing a sample blank extracting solution according to the pretreatment method in the step (3);
(4) Gradient elution on a chromatographic column: adopting a Phenomenex H18 chromatographic column (50mm x 3.00mm, 2.60 mu m), wherein the column temperature is 40 ℃, the flow rate is 0.40mL/min, and the sample injection volume is 2 mu L; the mobile phase A is a mixed solution of 5mmol/L ammonium formate and 0.05% formic acid aqueous solution in volume concentration, and the mobile phase B is methanol;
(5) Mass spectrometry analysis: an electrospray ion source is adopted, the flow rate of atomizing gas is 3.00L/min, the flow rate of drying gas is 15.00L/min, the temperature of a DL tube is 250 ℃, and a multi-reaction monitoring mode (MRM) is adopted;
(6) Determination of the standard curve:
mix standard stock solution: separately absorbing 100 mu L of single pesticide standard substance of methamidophos, aldicarb sulfoxide, aldicarb sulfone, monocrotophos, chlordimeform, 3-hydroxy carbofuran, aldicarb, phosphamidon, thiocyclam, phenthoate sulfoxide, carbofuran, phenthosulfonate, isocarbamate, phorate sulfoxide, metsulfuron, chlorsulfuron, metsulfuron, fensulfuron-methyl, demeton-o, demeton-s, terbufos sulfoxide, terbufos sulfone, ethoprophos, phenthoate, chlortriazophos, isofenphos-methyl, sulfotep-P, sulfothiotep, fon-methyl, phorate, terbufos, coumaphos, and acetonitrile to a constant volume of 10mL to obtain a mixed standard stock solution with a concentration of 10 mu g/mL, and storing in a refrigerator at 4 ℃;
pesticide substrate mixed standard working solution: diluting the mixed standard stock solution with the sample blank extract to prepare matrix mixed standard working solution of 0.01. Mu.g/mL, 0.02. Mu.g/mL, 0.04. Mu.g/mL, 0.1. Mu.g/mL and 0.8. Mu.g/mL, and performing on-machine measurement to generate a standard curve.
Preferably, the mass volume ratio of the Chinese medicinal material sample to be detected in the step (1) to water is 2: 9-10 g/mL; the mass volume ratio of the traditional Chinese medicine sample to be detected to the acetonitrile is 2: 9-10 g/mL.
Preferably, the extractant in the step (1) consists of the following raw materials in percentage by mass: 5.5g of anhydrous magnesium sulfate, 1.5g of sodium chloride, 0.5g of disodium hydrogen citrate and 1.0g of sodium citrate.
Preferably, the purifying agent in the step (1) is composed of the following raw materials in percentage by mass: 5 beads of 4mm zirconium oxide, 100mg of PSA and 600mg of anhydrous magnesium sulfate.
The oxidation pickaxe beads which are independently added into the sample play a role in auxiliary oscillation, and the sample is uniformly mixed; the zirconium oxide beads in the purifying agent also play a role in oscillation, and the added purifying agent reacts with the organic reagent to release heat, so that the effect of extraction and purification is prevented from being influenced by agglomeration.
Preferably, the oscillating in step (2) has a rotation speed of 1000RPM, and the time of each oscillation is 300S.
Preferably, the rotation speed of the centrifugation in the step (2) is 4000RPM, and the time of each centrifugation is 300S.
Preferably, the gradient elution procedure described in step (4) is 0.5 to 5.0min,10% by volume B; 5.0-8.0 min,95% by weight B;8.0 to 10min,10% by weight of B.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials, which takes a pharmacopoeia detection method as a comparison, optimizes a pretreatment purification step by selecting different extraction solvents and purification reagents, and improves the experimental efficiency; impurities are removed, damage to a chromatographic column and a mass spectrometer is reduced, and the accuracy and precision of a detection result are improved by optimizing the conditions of high performance liquid chromatography-tandem mass spectrometry. The invention has the advantages of shortened sample pretreatment time, high automation degree, detection time saving, great reduction of the use amount and the types of organic reagents, detection cost reduction, environmental friendliness, high detection sensitivity and data accuracy, more samples for one-time treatment and great improvement of detection efficiency. Proved by methodology, the recovery rate of the invention is within the range of 80-110%, and the precision is less than 10%.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials comprises the following steps:
(1) Preparing a sample solution: grinding semen euryales, weighing 2.0g of sample into a centrifuge tube, adding 9mL of water, uniformly mixing by vortex, adding 10mL of acetonitrile, and then adding an extracting agent (5.5 g of anhydrous magnesium sulfate, 1.5g of sodium chloride, 0.5g of disodium hydrogen citrate, 1.0g of sodium citrate), 24 zirconium beads and a purifying agent (5 zirconium oxide beads with the diameter of 4mm, 100mg of PSA and 600mg of anhydrous magnesium sulfate) to obtain a sample solution;
(2) Purifying: after the sample solution obtained in the step (1) is subjected to alternate oscillation centrifugation for 25min (wherein the oscillation rotating speed is 1000RPM, the time of each oscillation is 300S; the centrifugation rotating speed is 4000RPM, and the time of each centrifugation is 300S), purifying liquid is obtained, the purifying liquid is taken to pass through an organic microporous filter membrane with the diameter of 0.22 mu m, and the obtained filtrate is subjected to LC-MS/MS measurement;
(3) Mixing a sample blank extracting solution: taking a blank sample, and preparing a sample blank extracting solution according to the pretreatment method in the step (3);
(4) Gradient elution on a chromatographic column: adopting a Phenomenex H18 chromatographic column (50mm x 3.00mm, 2.60 mu m), wherein the column temperature is 40 ℃, the flow rate is 0.40mL/min, and the sample injection volume is 2 mu L; the mobile phase A is a mixed solution of 5mmol/L ammonium formate and 0.05% formic acid aqueous solution in volume concentration, and the mobile phase B is methanol; the gradient elution program is 0.5-5.0 min,10% B;5.0 to 8.0min,95 percent of B;8.0 to 10min,10 percent of the total weight of the crude oil;
(5) Mass spectrometry analysis: an electrospray ion source is adopted, the flow rate of atomizing gas is 3.00L/min, the flow rate of drying gas is 15.00L/min, the temperature of a DL tube is 250 ℃, and a multi-reaction monitoring mode (MRM) is adopted;
(6) Determination of the standard curve:
mix standard stock solutions: respectively sucking 100 mu L of single pesticide standard substance with the concentration of 1000 mu g/mL, fixing the volume to 10mL by using acetonitrile to obtain a mixed standard stock solution with the concentration of 10 mu g/mL, and storing in a refrigerator at 4 ℃;
pesticide substrate mixed standard working solution: diluting the mixed standard stock solution with the sample blank extract to prepare matrix mixed standard working solution of 0.01. Mu.g/mL, 0.02. Mu.g/mL, 0.04. Mu.g/mL, 0.1. Mu.g/mL and 0.8. Mu.g/mL, and performing on-machine measurement to generate a standard curve.
Table 1 is a standard curve for the pesticide components in example 1.
TABLE 1
Figure RE-GDA0003792990660000041
Figure RE-GDA0003792990660000051
Comparative example 1
Taking 3g of gordon euryale seed powder, precisely weighing, placing in a 50mL polystyrene centrifuge tube with a plug, adding 15mL of 1% glacial acetic acid solution, vortexing to fully infiltrate the powder, placing for 30 minutes, precisely adding 15mL of acetonitrile, vortexing and mixing uniformly, placing on an oscillator to shake vigorously for 5 minutes (500 times per minute), adding 7.5g of mixed powder (4: 1) of anhydrous magnesium sulfate and anhydrous sodium acetate, shaking immediately, placing on the oscillator to shake vigorously for 3 minutes (500 times per minute), cooling in a water bath for 10 minutes, centrifuging for 4000r/min for 5 minutes, taking 9mL of supernatant, placing in a dispersed solid phase extraction purification tube (900mg of anhydrous magnesium sulfate, 300mg of N-propylethylenediamine, 300mg of octadecylsilane bonded silica gel, 300mg of silica gel, 90mg of graphitized carbon black) which is filled with a purification material in advance, vortexing to fully mix uniformly, vortexing for 5 minutes (500 times per minute) on the oscillator to fully purify, centrifuging at a rotation speed of 4000r/min for 5 minutes, sucking 5mL of supernatant, placing on a nitrogen blowing instrument to 40 ℃ to obtain a filtrate, vortexing, concentrating, adding acetonitrile, and mixing uniformly, and obtaining a filtrate, and concentrating the filtrate at a temperature of 0.0.0.0 mL, and adding to obtain a concentrate.
The results of the tests of comparative example 1 and example 1 are shown in tables 2 and 3, respectively.
TABLE 2
Figure RE-GDA0003792990660000052
Figure RE-GDA0003792990660000061
TABLE 3
Figure RE-GDA0003792990660000062
Figure RE-GDA0003792990660000071
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 amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.

Claims (7)

1. A rapid detection method for 33 forbidden pesticide residues in traditional Chinese medicinal materials is characterized by comprising the following steps:
(1) Preparing a sample solution: crushing a traditional Chinese medicine sample to be detected into powder, sieving the powder by using a 80-mesh sieve, adding the powder into a centrifugal tube, adding water, adding acetonitrile after uniformly mixing the powder by vortex, and then adding an extracting agent, zirconium beads and a purifying agent to obtain a sample solution;
(2) Pretreatment: after the sample solution in the step (1) is subjected to alternate oscillation and centrifugation for 25min, purifying liquid is obtained, the purifying liquid is taken to pass through an organic microporous filter membrane with the diameter of 0.22 mu m, and the obtained filtrate is subjected to LC-MS/MS measurement;
(3) Mixing a sample blank extracting solution: taking a blank sample, and preparing a sample blank extracting solution according to the pretreatment method in the step (3);
(4) Gradient elution on a chromatographic column: adopting a Phenomenex H18 chromatographic column, wherein the column temperature is 40 ℃, the flow rate is 0.40mL/min, and the sample injection volume is 2 mu L; the mobile phase A is a mixed solution of 5mmol/L ammonium formate and 0.05% formic acid aqueous solution in volume concentration, and the mobile phase B is methanol;
(5) Mass spectrometry analysis: an electrospray ion source is adopted, the flow rate of atomizing gas is 3.00L/min, the flow rate of drying gas is 15.00L/min, the temperature of a DL tube is 250 ℃, and a multi-reaction monitoring mode is adopted;
(6) Determination of the standard curve:
mix standard stock solution: respectively absorbing 100 mu L of single pesticide standard substance of methamidophos, aldicarb sulfoxide, aldicarb sulfone, monocrotophos, chlordimeform, 3-hydroxy carbofuran, aldicarb, phosphamidon, thiocyclam, fenamiphos, carbofuran, fenamiphos, isocarbophos, phorate sulfoxide, metsulfuron-methyl, chlorsulfuron, metsulfuron-methyl, tribenuron-methyl, demeton-o, demeton-s, terbufos sulfoxide, terbufos sulfone, fenamiphos, chlordiazepoxide, methyl isoxathion, sulfotep, thiotep, fonofos, phorate, terbufos and coumaphos at the concentration of 1000 mu g/mL, fixing the volume to 10mL by using acetonitrile, obtaining a mixed standard solution with the concentration of 10 mu g/mL, and storing the mixed standard solution in a refrigerator at 4 ℃;
pesticide substrate mixed standard working solution: diluting the mixed standard stock solution with the sample blank extract, preparing matrix mixed standard working solutions of 0.01. Mu.g/mL, 0.02. Mu.g/mL, 0.04. Mu.g/mL, 0.1. Mu.g/mL and 0.8. Mu.g/mL respectively, and generating a standard curve after computer measurement.
2. The method for rapidly detecting 33 forbidden pesticide residues in the traditional Chinese medicinal materials according to claim 1, wherein the mass-to-volume ratio of the traditional Chinese medicinal material sample to be detected in the step (1) to water is 2:9-10 g/mL; the mass volume ratio of the Chinese medicinal material sample to be detected to the acetonitrile is 2:9-10 g/mL.
3. The method for rapidly detecting 33 forbidden pesticide residues in traditional Chinese medicinal materials according to claim 1, wherein the extracting agent in the step (1) is composed of the following raw materials in percentage by mass: 5.5g of anhydrous magnesium sulfate, 1.5g of sodium chloride, 0.5g of disodium hydrogen citrate and 1.0g of sodium citrate.
4. The method for rapidly detecting the residual of 33 forbidden pesticides in the traditional Chinese medicinal materials according to claim 1, wherein the purifying agent in the step (1) is prepared from the following raw materials in percentage by mass: 5 beads of 4mm zirconium oxide, 100mg PSA,600mg anhydrous magnesium sulfate.
5. The method for rapidly detecting 33 forbidden pesticide residues in the traditional Chinese medicinal materials according to claim 1, wherein the oscillating speed in the step (2) is 1000RPM, and the time of each oscillation is 300S.
6. The method for rapidly detecting 33 forbidden pesticide residues in the traditional Chinese medicinal materials according to claim 1, wherein the rotation speed of the centrifugation in the step (2) is 4000RPM, and the time of each centrifugation is 300S.
7. The method for rapidly detecting 33 prohibited pesticide residues in Chinese medicinal materials according to claim 1, wherein the gradient elution procedure in step (4) is 0.5-5.0 min, and the percent B is 10%; 5.0 to 8.0min,95 percent of B;8.0 to 10min,10% by weight of B.
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102854271A (en) * 2012-10-17 2013-01-02 国家烟草质量监督检验中心 Method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products
CN106290659A (en) * 2016-10-28 2017-01-04 陕西科技大学 Dispensed food for baby Pesticides and the Ultra Performance Liquid Chromatography level Four bar electrostatic field orbit ion trap mass spectrum screening method of veterinary drug
CN106324123A (en) * 2016-08-09 2017-01-11 国家烟草质量监督检验中心 Determination method of pesticide residual quantity in tobacco and tobacco products
CN111855871A (en) * 2020-07-30 2020-10-30 国家烟草质量监督检验中心 Method for measuring iprovalicarb and fluopyram in tobacco by combination of filtration type solid-phase extraction and supercritical fluid chromatography-mass spectrometry
US20210223219A1 (en) * 2018-04-16 2021-07-22 Chinese Academy Of Inspection And Quarantine Electronic id database and detection method for pesticide compound in edible agro-products based on lc-q-orbitrap
CN113156042A (en) * 2021-04-16 2021-07-23 陕西科技大学 Method for screening sulfonamide residues in goat milk
CN113376298A (en) * 2021-07-29 2021-09-10 天津市食品安全检测技术研究院 Method for rapidly determining residual quantity of 4 pesticides in rice
CN113945656A (en) * 2021-09-29 2022-01-18 中国农业科学院农产品加工研究所 Method for detecting pesticide and metabolite residues thereof in traditional Chinese medicinal materials
KR20220018154A (en) * 2020-08-06 2022-02-15 대한민국(국립농산물품질관리원장) Analytical method for dithiocarbamate pesticide remaining on agricultural product

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102854271A (en) * 2012-10-17 2013-01-02 国家烟草质量监督检验中心 Method for measuring residues of three phenoxy carboxylic acid pesticides in tobacco and tobacco products
CN106324123A (en) * 2016-08-09 2017-01-11 国家烟草质量监督检验中心 Determination method of pesticide residual quantity in tobacco and tobacco products
CN106290659A (en) * 2016-10-28 2017-01-04 陕西科技大学 Dispensed food for baby Pesticides and the Ultra Performance Liquid Chromatography level Four bar electrostatic field orbit ion trap mass spectrum screening method of veterinary drug
US20210223219A1 (en) * 2018-04-16 2021-07-22 Chinese Academy Of Inspection And Quarantine Electronic id database and detection method for pesticide compound in edible agro-products based on lc-q-orbitrap
CN111855871A (en) * 2020-07-30 2020-10-30 国家烟草质量监督检验中心 Method for measuring iprovalicarb and fluopyram in tobacco by combination of filtration type solid-phase extraction and supercritical fluid chromatography-mass spectrometry
KR20220018154A (en) * 2020-08-06 2022-02-15 대한민국(국립농산물품질관리원장) Analytical method for dithiocarbamate pesticide remaining on agricultural product
CN113156042A (en) * 2021-04-16 2021-07-23 陕西科技大学 Method for screening sulfonamide residues in goat milk
CN113376298A (en) * 2021-07-29 2021-09-10 天津市食品安全检测技术研究院 Method for rapidly determining residual quantity of 4 pesticides in rice
CN113945656A (en) * 2021-09-29 2022-01-18 中国农业科学院农产品加工研究所 Method for detecting pesticide and metabolite residues thereof in traditional Chinese medicinal materials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张立田 等: "液相色谱串联质谱法测定青贮玉米中氨基甲酸酯类农药残留", 《饲料研究》, vol. 42, no. 8, pages 79 - 82 *

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