CN105866272A - A method of detecting pesticide residues in a healthcare product - Google Patents

A method of detecting pesticide residues in a healthcare product Download PDF

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Publication number
CN105866272A
CN105866272A CN201610195036.9A CN201610195036A CN105866272A CN 105866272 A CN105866272 A CN 105866272A CN 201610195036 A CN201610195036 A CN 201610195036A CN 105866272 A CN105866272 A CN 105866272A
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detection
sample
pesticide residues
health product
prepared
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CN201610195036.9A
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王群
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Qingdao Samcdc Public Health Inspection Co Ltd
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Qingdao Samcdc Public Health Inspection Co Ltd
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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
    • G01N2030/025—Gas 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

Abstract

The invention belongs to the technical field of pesticide residue detection, and relates to a method of detecting pesticide residues in a healthcare product. A detection process includes sample preparation, GC-MS detection and LC-MS/MS verification. The method includes subjecting the healthcare product and acetonitrile to ultrasonic wave processing or homogenizing, centrifuging by adopting anhydrous magnesium sulfate, anhydrous sodium acetate and an adsorbent to extract a detection sample, subjecting the detection sample to vacuum concentration until the sample is dry, adding acetone, dissolving with a vortex machine and an ultrasonic cleaner, filtering with an organic phase filtration membrane to obtain a solution for GC-MS detection, and when the GC-MS detection result shows that the detection sample contains the pesticide residues, filtering with the organic phase filtration membrane to obtain a solution for LC-MS/MS verification to verify whether the detection sample contains the pesticide residues. The method rapidly and accurately detects the pesticide residues in the healthcare product through adopting the GC-MS and the LC-MS/MS, reduces consumption of organic solvents, and is good in reproducibility, simple in detection process, scientific and reasonable in principles, convenient in operation, safe, reliable, low in detection cost, accurate in result and environmental friendly.

Description

A kind of detection method of health product Pesticide Residues
Technical field:
The invention belongs to the Detection Technologies of Pesticide Residues field, relate to a kind of health product Pesticide Residues Detection method, use GC-MS (gas chromatography-mass spectrum) and LC-MS/MS (liquid chromatograph- Mass spectrum/mass spectrum) quickly, accurately detect the persticide residue in health product, reduce organic reagent Consume, favorable reproducibility.
Background technology:
Health product are the popular sayings of health food, and the nutrient substance wanted according to needed by human body becomes Part, extract from Matter Compositions such as natural plants, veterinary antibiotics and milk product and be made, right Mending three aspects classification preparations by clear, mediation for the use of human body, the health care of health food is made With in present day society, the most progressively accepted by broad masses, although can not be the shortest Improve the body constitution of people in time, but take for a long time and can make people's life lengthening.Health food former Material composition has various ways, and the building form with crops as raw material inevitably exists agriculture The problem of medicine residual, the harm of pesticide residues mainly has three aspects: one is edible containing a large amount of high The food of poison, highly toxic pesticide residual can cause acute poisoning accident, is eaten for a long time pesticide residues and surpasses Target agricultural byproducts, may cause chronic poisoning, cause the generation of disease, even have influence on down A generation；Two is unreasonable use pesticide, particularly herbicide, causes phytotoxicity accident frequent, draws Rising drops in production over a large area even has no harvest, and has a strong impact on agricultural production；Three is that countries in the world are to agricultural and sideline product The limit standard regulation of product Pesticide Residues is increasingly stricter, with Pesticide Residue as art wall Building, limit agricultural byproducts import, protecting agriculture produces.In the prior art, detection pesticide is residual The method stayed is to utilize Organophosphorus and carbamate pesticides class medicine to cholinester under certain condition The inhibitory action of enzyme normal function, judges pesticide residues by suppression ratio.Health product exist agriculture Medicine residual not only cannot play the effect of health care, and health product can be caused to pollute, and harm uses The health of person, even threat to life, at present, various documents, report and market do not have It is specifically designed for the detection of health product Pesticide Residues.Therefore, research and development one quick and precisely, operation The detection method of health product Pesticide Residues easy and with low cost, food for preventing security incident Generation, it is ensured that health product effectively play its effect, have good society and economic worth, Have a extensive future.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming prior art to exist, design is a kind of the most accurate Really, the detection method of health product Pesticide Residues easy and simple to handle and with low cost, food for preventing The generation of security incident, it is ensured that health product effectively play its effect.
To achieve these goals, the detection method of the health product Pesticide Residues that the present invention relates to Characterization processes process include sample prepare, GC-MS detection and LC-MS/MS checking totally three Step:
(1), prepared by sample: 2.0g health product and 10ml acetonitrile are placed in capacity is 50ml A PP centrifuge tube after ultrasonic echography 20min or homogenizing 1min, then that 6g is anhydrous Magnesium sulfate and 1.5g anhydrous sodium acetate add a PP centrifuge tube, rock number PP of vibration from With the centrifugation 3min of 4000rpm after heart pipe 5-8min, pouring out supernatant addition capacity is In No. two PP centrifuge tubes of 50ml, then by 1.5g anhydrous magnesium sulfate, 1.0g C18 adsorbent, 1.0g PSA adsorbent and 1.0g Graphon adsorbent also add in No. two PP centrifuge tubes, By after No. two PP centrifuge tube vortex 1min with the centrifugation 3min of 4000rpm, pour out Clear liquid is standby, prepared by the sample completing detection；
(2), GC-MS detection: measure detection sample prepared by 5mL step (1) at 30-35 DEG C Lower concentrating under reduced pressure is spin-dried for, and adds 1ml acetone and obtain mixture in residue, with vortice with super Sound wave cleaning machine by mixture dissolve after with the organic facies membrane filtration of 0.22 μm obtain molten Liquid detects solution as GC-MS, and the chromatographic column in GC-MS detection is HP-5ms, and thickness is 250um, a length of 30m, a diameter of 0.25mm, delivery gas is helium, and flow rate of carrier gas is 1.20mL/min, the gas phase testing time is 27.2min, column oven heating schedule such as following table:
Speed Final temperature Retention time
- 70℃ 1min
25℃/min 180℃ 0min
10℃/min 280℃ 10min
Result shows the corresponding target compound monitoring ion phase one occurred in retention time and set The peak caused, and consistent with target monitoring ion ratio, show to detect containing pesticide residues in sample, Complete GC-MS detection；
(3), LC-MS/MS checking: when the testing result of step (2) contains for detecting in sample When having pesticide residues, measure detection sample prepared by 1mL step (1), use 0.22 μm Organic facies membrane filtration sample after as LC-MS/MS checking solution, LC-MS/MS detect In chromatographic column be 120EC-C18, the size of chromatographic column is 100mm*3.0mm and 2.7 μm, The column temperature of chromatographic column is 40 DEG C, the corresponding target compound occurring in retention time with setting The peak that ion pair and ion ratio etc. are consistent, confirms in detection sample containing pesticide residues, complete Becoming LC-MS/MS checking, wherein retention time is ± 0.1min.
The health product of the detection that the present invention relates to are the health product sold on market；Pesticide residues Including parathion-methyl, Malathion, fenifrothion, chlopyrifos, parathion, three chlorbensides Alcohol, isocarbophos, Isofenphos methyl, ethiprole, procymidone, Profenofos, triazophos, connection Benzene chrysanthemum ester, Fenpropathrin, RP-26019, lambda-cyhalothrin, pyridaben, cyfloxylate, chlorine Cyano chrysanthemate, flucythrinate, fenvalerate, taufluvalinate, decis, pentachloro-nitro Benzene, diazinon, vinclozolin, Bravo, thimet, triazolone, carbaryl, α- Gamma Hexaochlorocyclohexane, Β-Gamma Hexaochlorocyclohexane, Δ-Gamma Hexaochlorocyclohexane, Γ-Gamma Hexaochlorocyclohexane, heptachlor, O, P-DDT, P, P-DDT, P, P-DDD, atrazine, fenthion, drinox, Buprofezin, edifenphos, trans-Niran, suitable -Niran, metalaxyl, quintiofos, Permethrin, paclobutrazol, Nemacur, Triadimenol, Shuan Jia Amidine, endrin, dieldrin, 3-hydroxyl carbofuran, avilamycin, orthene, pyridine Worm amidine, Aldicarb, Hexythiazox, butachlor, carbaryl, carbendazim, carbofuran, fourth sulfur gram Budweiser, d ichlorbenzuron, cyromazine, dichlorvos, Difenoconazole, diflubenzuron, Rogor, alkene acyl Morpholine, edifenphos, phonamiphos, Nemacur, imidacloprid, Bayer 71628, Methomyl, meta-tolyl-N-methylcarbamate (MTMC), Azodrin, omethoate, paclobutrazol, thimet, Phosalone, phosmet, phoxim, Pyrimethanil, triazolone and metrifonate；The equipment that detection uses is the equipment of the detection of routine.
The present invention compared with prior art, uses GC-MS and LC-MS/MS quickly, accurately examine Survey the pesticide residues in health product, reduce organic reagent consumption, favorable reproducibility；Its characterization processes Simply, scientific in principle is reasonable, and easy to operate, safe and reliable, testing cost is low, and result is accurate, Use environmental friendliness.
Detailed description of the invention:
Below by embodiment, the present invention is described further.
Embodiment:
The characterization processes process of the detection method of the health product Pesticide Residues that the present embodiment relates to Prepare including sample, GC-MS detects and LC-MS/MS checking three steps totally:
(1), prepared by sample: 2.0g health product and 10ml acetonitrile are placed in capacity is 50ml A PP centrifuge tube after ultrasonic echography 20min or homogenizing 1min, then that 6g is anhydrous Magnesium sulfate and 1.5g anhydrous sodium acetate add a PP centrifuge tube, rock number PP of vibration from With the centrifugation 3min of 4000rpm after heart pipe 5-8min, pouring out supernatant addition capacity is In No. two PP centrifuge tubes of 50ml, then by 1.5g anhydrous magnesium sulfate, 1.0g Cleanert S C18 adsorbent, 1.0g Cleanert PSA adsorbent and 1.0g Graphon adsorbent are also Add in No. two PP centrifuge tubes, by after No. two PP centrifuge tube vortex 1min with 4000rpm's Centrifugation 3min, pours out supernatant standby, prepared by the sample completing detection；
(2), GC-MS detection: measure detection sample prepared by 5mL step (1) at 30-35 DEG C Lower concentrating under reduced pressure is spin-dried for, and adds 1ml acetone and obtain mixture in residue, with vortice with super Sound wave cleaning machine by mixture dissolve after with the organic facies membrane filtration of 0.22 μm obtain molten Liquid detects solution as GC-MS, and the chromatographic column in GC-MS detection is HP-5ms, and thickness is 250um, a length of 30m, a diameter of 0.25mm, delivery gas is He (helium), carrier gas Flow velocity is 1.20mL/min, and the gas phase testing time is 27.2min, and column oven heating schedule is as follows Table:
Speed Final temperature Retention time
- 70℃ 1min
25℃/min 180℃ 0min
10℃/min 280℃ 10min
Result shows the corresponding target compound monitoring ion phase one occurred in retention time and set The peak caused, and consistent with target monitoring ion ratio, show to detect containing pesticide residues in sample, Complete GC-MS detection；
(3), LC-MS/MS checking: when the testing result of step (2) contains for detecting in sample When having pesticide residues, measure detection sample prepared by 1mL step (1), use 0.22 μm Organic facies membrane filtration sample after as LC-MS/MS checking solution, LC-MS/MS detect In chromatographic column be Agilent poroshell 120EC-C18, the size of chromatographic column is 100mm*3.0mm and 2.7 μm, the column temperature of chromatographic column is 40 DEG C, in retention time occur with The consistent peaks such as the corresponding target compound ion pair set and ion ratio, confirm detection sample Containing pesticide residues in product, completing LC-MS/MS checking, wherein retention time is ± 0.1min.
The health product of the detection related in the present embodiment are the health product sold on market；Pesticide Residual includes parathion-methyl, Malathion, fenifrothion, chlopyrifos, parathion, trichlorine Qikron, isocarbophos, Isofenphos methyl, ethiprole, procymidone, Profenofos, triazophos, Biphenthrin, Fenpropathrin, RP-26019, lambda-cyhalothrin, pyridaben, cyfloxylate, Cypermethrin, flucythrinate, fenvalerate, taufluvalinate, decis, pentachloro-nitre Base benzene, diazinon, vinclozolin, Bravo, thimet, triazolone, carbaryl, α -Gamma Hexaochlorocyclohexane, Β-Gamma Hexaochlorocyclohexane, Δ-Gamma Hexaochlorocyclohexane, Γ-Gamma Hexaochlorocyclohexane, heptachlor, O, P-DDT, P, P-DDT, P, P-DDD, atrazine, fenthion, drinox, Buprofezin, edifenphos, trans-Niran, suitable -Niran, metalaxyl, quintiofos, Permethrin, paclobutrazol, Nemacur, Triadimenol, Shuan Jia Amidine, endrin, dieldrin, 3-hydroxyl carbofuran, avilamycin, orthene, pyridine Worm amidine, Aldicarb, Hexythiazox, butachlor, carbaryl, carbendazim, carbofuran, fourth sulfur gram Budweiser, d ichlorbenzuron, cyromazine, dichlorvos, Difenoconazole, diflubenzuron, Rogor, alkene acyl Morpholine, edifenphos, phonamiphos, Nemacur, imidacloprid, Bayer 71628, Methomyl, meta-tolyl-N-methylcarbamate (MTMC), Azodrin, omethoate, paclobutrazol, thimet, Phosalone, phosmet, phoxim, Pyrimethanil, triazolone and metrifonate；The equipment that detection uses is the equipment of the detection of routine.

Claims (2)

1. the detection method of a health product Pesticide Residues, it is characterised in that characterization processes mistake Journey includes that prepared by sample, GC-MS detects and LC-MS/MS checking three steps totally:
(1), prepared by sample: 2.0g health product and 10ml acetonitrile are placed in capacity is 50ml A PP centrifuge tube after ultrasonic echography 20min or homogenizing 1min, then that 6g is anhydrous Magnesium sulfate and 1.5g anhydrous sodium acetate add a PP centrifuge tube, rock number PP of vibration from With the centrifugation 3min of 4000rpm after heart pipe 5-8min, pouring out supernatant addition capacity is In No. two PP centrifuge tubes of 50ml, then by 1.5g anhydrous magnesium sulfate, 1.0g C18 adsorbent, 1.0g PSA adsorbent and 1.0g Graphon adsorbent also add in No. two PP centrifuge tubes, By after No. two PP centrifuge tube vortex 1min with the centrifugation 3min of 4000rpm, pour out Clear liquid is standby, prepared by the sample completing detection；
(2), GC-MS detection: measure detection sample prepared by 5mL step (1) at 30-35 DEG C Lower concentrating under reduced pressure is spin-dried for, and adds 1ml acetone and obtain mixture in residue, with vortice with super Sound wave cleaning machine by mixture dissolve after with the organic facies membrane filtration of 0.22 μm obtain molten Liquid detects solution as GC-MS, and the chromatographic column in GC-MS detection is HP-5ms, and thickness is 250um, a length of 30m, a diameter of 0.25mm, delivery gas is helium, and flow rate of carrier gas is 1.20mL/min, the gas phase testing time is 27.2min, column oven heating schedule such as following table:
Result shows the corresponding target compound monitoring ion phase one occurred in retention time and set The peak caused, and consistent with target monitoring ion ratio, show to detect containing pesticide residues in sample, Complete GC-MS detection；
(3), LC-MS/MS checking: when the testing result of step (2) contains for detecting in sample When having pesticide residues, measure detection sample prepared by 1mL step (1), use 0.22 μm Organic facies membrane filtration sample after as LC-MS/MS checking solution, LC-MS/MS detect In chromatographic column be 120EC-C18, the size of chromatographic column is 100mm*3.0mm and 2.7 μm, The column temperature of chromatographic column is 40 DEG C, the corresponding target compound occurring in retention time with setting The peak that ion pair and ion ratio etc. are consistent, confirms in detection sample containing pesticide residues, complete Becoming LC-MS/MS checking, wherein retention time is ± 0.1min.
The detection method of health product Pesticide Residues the most according to claim 1, it is special Levying the health product being to detect is the health product sold on market；Pesticide residues include methyl pair Sulfur phosphorus, Malathion, fenifrothion, chlopyrifos, parathion, dicofol, water amine sulfur Phosphorus, Isofenphos methyl, ethiprole, procymidone, Profenofos, triazophos, Biphenthrin, first Cyano chrysanthemate, RP-26019, lambda-cyhalothrin, pyridaben, cyfloxylate, cypermethrin, fluorine Fenvalerate, fenvalerate, taufluvalinate, decis, pentachloronitrobenzene, diazinon, Vinclozolin, Bravo, thimet, triazolone, carbaryl, α-Gamma Hexaochlorocyclohexane, Β- Gamma Hexaochlorocyclohexane, Δ-Gamma Hexaochlorocyclohexane, Γ-Gamma Hexaochlorocyclohexane, heptachlor, O, P-DDT, P, P-DDT, P, P-DDD, Atrazine, fenthion, drinox, Buprofezin, edifenphos, trans-Niran, cis-Niran, first Frost spirit, quintiofos, Permethrin, paclobutrazol, Nemacur, Triadimenol, Amitraz, different Di Shi Agent, dieldrin, 3-hydroxyl carbofuran, avilamycin, orthene, Acetamiprid, tears go out Prestige, Hexythiazox, butachlor, carbaryl, carbendazim, carbofuran, carbosulfan, children of going out Urea, cyromazine, dichlorvos, Difenoconazole, diflubenzuron, Rogor, dimethomorph, enemy's pestilence Phosphorus, phonamiphos, Nemacur, imidacloprid, Bayer 71628, Methomyl, meta-tolyl-N-methylcarbamate (MTMC), Azodrin, Omethoate, paclobutrazol, thimet, Phosalone, phosmet, phoxim, pyrimethanil, Triazolone and metrifonate；The equipment that detection uses is the equipment of the detection of routine.
CN201610195036.9A 2016-03-31 2016-03-31 A method of detecting pesticide residues in a healthcare product Pending CN105866272A (en)

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CN107505421A (en) * 2017-09-25 2017-12-22 重庆市农业科学院 The rapid extraction and purification method of ethiprole and its metabolite residue in a kind of birds, beasts and eggs
CN107860841A (en) * 2017-11-06 2018-03-30 舟山市食品药品检验检测研究院 A kind of method of ethiprole and its metabolin in detection birds, beasts and eggs
CN108226343A (en) * 2018-01-08 2018-06-29 中国检验检疫科学研究院综合检测中心 Multiple Pesticides method for detecting residue in a kind of vegetables and fruits
CN108508130A (en) * 2018-04-11 2018-09-07 国家烟草质量监督检验中心 A kind of method that ultra high efficiency conjunction phase chromatography-tandem mass spectrum technology splits, measures Chiral pesticide metalaxyl and dimethomorph enantiomer
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US10849600B2 (en) 2016-03-08 2020-12-01 Entech Instruments Inc. Breath condensate and saliva analysis using oral rinse
US10502664B2 (en) 2016-03-08 2019-12-10 Entech Instruments Inc. Vacuum-assisted sample extraction device and method
CN107037149A (en) * 2017-04-08 2017-08-11 中国热带农业科学院农产品加工研究所 Ethiprole and its metabolite residue amount method for measuring in a kind of egg
CN107037149B (en) * 2017-04-08 2019-09-20 中国热带农业科学院农产品加工研究所 Fipronil and its metabolite residue amount method for measuring in a kind of egg
CN107505421A (en) * 2017-09-25 2017-12-22 重庆市农业科学院 The rapid extraction and purification method of ethiprole and its metabolite residue in a kind of birds, beasts and eggs
CN107860841A (en) * 2017-11-06 2018-03-30 舟山市食品药品检验检测研究院 A kind of method of ethiprole and its metabolin in detection birds, beasts and eggs
CN107860841B (en) * 2017-11-06 2020-07-24 舟山市食品药品检验检测研究院 Method for detecting fipronil and its metabolite in poultry egg
CN108226343A (en) * 2018-01-08 2018-06-29 中国检验检疫科学研究院综合检测中心 Multiple Pesticides method for detecting residue in a kind of vegetables and fruits
US11896366B2 (en) 2018-03-06 2024-02-13 Entech Instruments Inc. Ventilator-coupled sampling device and method
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Application publication date: 20160817