CN108152395A - A kind of method for measuring pesticide residue in agricultural products - Google Patents
A kind of method for measuring pesticide residue in agricultural products Download PDFInfo
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- CN108152395A CN108152395A CN201711320979.0A CN201711320979A CN108152395A CN 108152395 A CN108152395 A CN 108152395A CN 201711320979 A CN201711320979 A CN 201711320979A CN 108152395 A CN108152395 A CN 108152395A
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- agricultural products
- pesticide residue
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The present invention relates to a kind of methods for measuring pesticide residue in agricultural products, belong to technical field of analytical chemistry.The method of the invention includes sample pre-treatments step；The sample pre-treatments step includes extraction step, purifying step；The extraction step is：Agricultural product are dissolved, homogeneous, centrifuged, isolated sample to be clean；The purifying step is：It is purified using solid phase extraction column.Present invention obtains satisfied separating effects and detection sensitivity.
Description
Technical field
The present invention relates to a kind of methods for measuring pesticide residue in agricultural products, belong to technical field of analytical chemistry.
Background technology
Pesticide mean for prevent endanger agriculture forest and husbandry production harmful organism and coordinate plant growth chemicals and
Biologics.Usually the various auxiliary agents for health and improvement active ingredient physico-chemical property are also included within interior.
According to toxicity overall merit (acute oral, percutaneous toxicity, the chronic toxicity of common pesticides in agricultural production (active compound)
Deng), it is divided into high poison, medium poison, less toxic three classes.
High-toxic pesticide (LD50<50mg/kg)：There are 3911, Soviet Unionization 203,1605, parathion-methyl, 1059, chlorfenvinpho, long effect
Phosphorus, phosphamidon, acephatemet, isothioate, carbophenothion, flolimat, zinc phosphide, aluminum phosphate, cyanide, Furadan, Fluorakil 100, arsenic
Frost, Spanon, ethylmercuric cloride, phenylmercuric acetate, ulcer are net, chloropicrin, pentachlorophenol, dibromochloropropane, 401 etc..
Medium poison pesticide (LD50 is between 50-500mg/kg)：There are Folithion, Rogor, phenthoate dimephenthoate cidial, Ethodan, imines sulphur
Phosphorus, Nankor, six six six, fortified benzene hexachloride, toxaphene, Niran, DDT, sevin, Hopside, isoprocarb, MTMC,
Dimethyl phenyl carbamate, Aphox, Entex, DDVP, pyrethroid, Hinosan, kitazine, fenaminosulf, 402, asomate, rice foot
Blueness, Tuzet, for gloomy amine, milneb, 2,4- drops, Avadex, propachlor etc..
Low-toxin farm chemicals (LD50>500mg/kg)：Have metrifonate, marathon, orthene, phoxim, dicofol,
Carbendazim, thiophanate, captan, zineb, thiram, carboxin, different careless pest are net, aliette, Bravo, nitrofen, propanil,
Atrazine, Machete, drag-line, benthiocarb, 2 first, 4 chlorine, chlortoluron, diuron, trefanocide, Bentazon, Dalapon, glyphosate
Deng.
Pesticide poisoning the lighter shows as headache, giddy, nausea, burnout, abdominal pain etc., and spasm, expiratory dyspnea, dusk occurs in severe one
Fan, gatism or even death.
The nitrate of human body intake has 81.2% from contaminated vegetables, and nitrate is both at home and abroad generally acknowledged three substantially
The precursor of cancer object nitrosamine.
The heavy metal elements such as mercury, arsenic, lead, cadmium in municipal refuse, sewage and chemical phosphatic ferfilizer are nervous system, breathing system
The important carcinogen of system, excretory system.
Organo-chlorine pesticide is accumulated in body fat, the enzyme of induced liver, is one of hepatic sclerosis enlargement reason.
Habitual headache, dizzy, weak, hidrosis, depression, failure of memory, alopecia, weak etc. are the hidden of toxic vegetables
Property effect, be the omen for causing the diseases such as various cancers.
Contaminated vegetables are eaten for a long time, are to lead to cancer, artery sclerosis, cardiovascular disease, fetal anomaly, stillborn foetus, early die young, is early
(vast majority of people does not show symptom to the major reason for the diseases such as decline at once after eating harmful vegetables, and poisonous substance is rich in human body
Collection, the time, which has been grown, will lead to serious consequence).
Invention content
The method that the present invention uses Solid Phase Extraction pre-treatment combination liquid chromatogram, establishes the survey of pesticide in a variety of agricultural product
Determine method, solve the defects of existing method is to a variety of pesticide residue in agricultural products qualitative and quantitative analyses.
The present invention provides a kind of methods for measuring pesticide residue in agricultural products, and the method includes sample pre-treatments steps
Suddenly；
The sample pre-treatments step includes extraction step, purifying step；
The extraction step is：Agricultural product are dissolved, homogeneous, centrifuged, isolated sample to be clean；
The purifying step is：It is purified using solid phase extraction column.
The lysate of agricultural product of the present invention is preferably：Water and dichloromethane or water or aqueous acetone solution.
The method of the invention preferably comprises liquid chromatographic detection step；
Chromatographic condition：
Chromatographic column：Silicagel column；
Mobile phase：Mobile phase A：Water, Mobile phase B：Acetonitrile；
Isocratic elution：30-50%A.
The specification of chromatographic column of the present invention is preferably：2mm×80-100mm.
The granularity of stationary phase of the present invention is preferably 5-8 μm.
The flow velocity of mobile phase of the present invention is preferably 0.2-0.25mL/min.
The column temperature of chromatographic column of the present invention is preferably 35-45 DEG C.
Sampling volume of the present invention is preferably 10-15 μ L.
The method of the invention includes sample pre-treatments step；The sample pre-treatments step includes extraction step, purification
Step；The extraction step is：Agricultural product are dissolved, homogeneous, centrifuged, isolated sample to be clean；The purifying step is：
It is purified using solid phase extraction column.Obtain satisfied separating effect and detection sensitivity.Existing method is solved to a variety of agricultures
In product the defects of persticide residue qualitative and quantitative analysis.
Specific embodiment
Following non-limiting examples can make those of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Embodiment 1
A kind of method for measuring pesticide residue in agricultural products, described method includes following steps：
Sample pre-treatments step：
Extraction step：10g pineapple samples are added in the mixed liquor of 30mL water and 30mL dichloromethane, 20000r/min
Homogeneous 2min, 5000r/min centrifugation 5min, separation supernatant obtain sample to be clean；
Purifying step：Solid phase extraction column is first eluted using 5mL ethyl alcohol, 5mL water in advance successively, adds sample to be clean,
3mL water, the elution of 3mL methanol is respectively adopted, is then eluted using 2mL3% ammoniated methanols solution, collects eluent, it is dry, it uses
Flow phased soln；
Liquid chromatographic detection step：
Chromatographic condition：
Chromatographic column：Silicagel column (2mm × 100mm, 5 μm)；
Mobile phase：Mobile phase A：Water, Mobile phase B：Acetonitrile；
Isocratic elution：50%A；
The flow velocity of mobile phase is 0.22mL/min；
The column temperature of chromatographic column is 40 DEG C；
Sampling volume is 10 μ L.
Quantifying for pineapple sample is limited to 0.008mg/kg.
Embodiment 2
A kind of method for measuring pesticide residue in agricultural products, described method includes following steps：
Sample pre-treatments step：
Extraction step：1g Longjing tea samples are added in 20mL water, 20000r/min homogeneous 2min, 5000r/min
5min is centrifuged, supernatant is detached, adds in isometric dichloromethane, is extracted, is discarded dichloromethane layer and obtain sample to be clean；
Purifying step：Solid phase extraction column is first eluted using 5mL ethyl alcohol, 5mL water in advance successively, adds sample to be clean,
Using 3mL water elutions, eluent is collected；
Liquid chromatographic detection step：
Chromatographic condition：
Chromatographic column：Silicagel column (2mm × 100mm, 5 μm)；
Mobile phase：Mobile phase A：Water, Mobile phase B：Acetonitrile；
Isocratic elution：30%A；
The flow velocity of mobile phase is 0.22mL/min；
The column temperature of chromatographic column is 40 DEG C；
Sampling volume is 10 μ L.
Quantifying for Longjing tea sample is limited to 0.015mg/kg.
Embodiment 3
A kind of method for measuring pesticide residue in agricultural products, described method includes following steps：
Sample pre-treatments step：
Extraction step：2g corn samples are added in 20mL 25v/v% aqueous acetone solutions, 20000r/min homogeneous
2min, 5000r/min centrifuge 5min, detach supernatant, add in isometric dichloromethane, extract, discard dichloromethane layer and obtain
Sample to be clean；
Purifying step：Solid phase extraction column is first eluted using 5mL ethyl alcohol, 5mL water in advance successively, adds sample to be clean,
3mL water, the elution of 3mL methanol is respectively adopted, is then eluted using 2mL3% ammoniated methanols solution, collects eluent, it is dry, it uses
Flow phased soln；
Liquid chromatographic detection step：
Chromatographic condition：
Chromatographic column：Silicagel column (2mm × 100mm, 5 μm)；
Mobile phase：Mobile phase A：Water, Mobile phase B：Acetonitrile；
Isocratic elution：50%A；
The flow velocity of mobile phase is 0.22mL/min；
The column temperature of chromatographic column is 40 DEG C；
Sampling volume is 10 μ L.
Quantifying for corn sample is limited to 0.008mg/kg.
Claims (8)
- A kind of 1. method for measuring pesticide residue in agricultural products, it is characterised in that：The method includes sample pre-treatments steps；The sample pre-treatments step includes extraction step, purifying step；The extraction step is：Agricultural product are dissolved, homogeneous, centrifuged, isolated sample to be clean；The purifying step is：It is purified using solid phase extraction column.
- 2. the method for pesticide residue in agricultural products is measured according to claim 1, it is characterised in that：The agricultural product it is molten Solving liquid is：Water and dichloromethane or water or aqueous acetone solution.
- 3. the method for pesticide residue in agricultural products is measured according to claim 2, it is characterised in that：The method includes liquid Phase chromatography detecting step；Chromatographic condition：Chromatographic column：Silicagel column；Mobile phase：Mobile phase A：Water, Mobile phase B：Acetonitrile；Isocratic elution：30-50%A.
- 4. the method for pesticide residue in agricultural products is measured according to claim 3, it is characterised in that：The rule of the chromatographic column Lattice are：2mm×80-100mm.
- 5. the method for pesticide residue in agricultural products is measured according to claim 4, it is characterised in that：The granularity of stationary phase is 5-8μm。
- 6. the method for pesticide residue in agricultural products is measured according to claim 5, it is characterised in that：The stream of the mobile phase Speed is 0.2-0.25mL/min.
- 7. the method for pesticide residue in agricultural products is measured according to claim 6, it is characterised in that：The column of the chromatographic column Temperature is 35-45 DEG C.
- 8. the method for pesticide residue in agricultural products is measured according to claim 7, it is characterised in that：Sampling volume is 10- 15μL。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711320979.0A CN108152395A (en) | 2017-12-12 | 2017-12-12 | A kind of method for measuring pesticide residue in agricultural products |
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| CN201711320979.0A CN108152395A (en) | 2017-12-12 | 2017-12-12 | A kind of method for measuring pesticide residue in agricultural products |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110824090A (en) * | 2019-11-27 | 2020-02-21 | 日照健安检测技术服务有限公司 | Method for rapidly detecting residual quantity of fosetyl-aluminum in vegetables |
| CN111272907A (en) * | 2020-04-02 | 2020-06-12 | 哈尔滨海关技术中心 | Method for determining residual quantity of bentazone in plant source food by liquid chromatography-mass spectrometry/mass spectrometry |
| CN113686988A (en) * | 2021-08-19 | 2021-11-23 | 山东省环境保护科学研究设计院有限公司 | Method for detecting bactericide in solid waste |
| CN114910588A (en) * | 2022-05-13 | 2022-08-16 | 厦门泓益检测有限公司 | Synchronous detection method for dalapon, dicamba, pentol, acantol and toxigenin in tea |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105116064A (en) * | 2015-07-17 | 2015-12-02 | 中国农业科学院茶叶研究所 | Automatic sample pretreatment and detection method for detecting residual of multiple pesticides in tea leaves |
-
2017
- 2017-12-12 CN CN201711320979.0A patent/CN108152395A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105116064A (en) * | 2015-07-17 | 2015-12-02 | 中国农业科学院茶叶研究所 | Automatic sample pretreatment and detection method for detecting residual of multiple pesticides in tea leaves |
Non-Patent Citations (3)
| Title |
|---|
| CARLO BICCHI等: "HPLC-UV Determination of Pesticide Residues at 0.01ppm in Apple and Pear Pulp used for Baby Food", 《J. HIGH RESOL. CHROMATOGR》 * |
| HUI-LI WANG 等: "Pyraflufen-ethyl Residues in Soil by Solid Phase Extraction and High-Performance Liquid Chromatography with UV Detection", 《ANALYTICAL SCIENCES DECEMBER》 * |
| 朱春红: "小麦中三嗪类除草剂多残留的液相色谱测定方法研究", 《中国优秀硕士学位论文全文数据库 农业科技辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110824090A (en) * | 2019-11-27 | 2020-02-21 | 日照健安检测技术服务有限公司 | Method for rapidly detecting residual quantity of fosetyl-aluminum in vegetables |
| CN111272907A (en) * | 2020-04-02 | 2020-06-12 | 哈尔滨海关技术中心 | Method for determining residual quantity of bentazone in plant source food by liquid chromatography-mass spectrometry/mass spectrometry |
| CN111272907B (en) * | 2020-04-02 | 2022-07-01 | 哈尔滨海关技术中心 | Method for determining residual quantity of bentazone in plant source food by liquid chromatography-mass spectrometry/mass spectrometry |
| CN113686988A (en) * | 2021-08-19 | 2021-11-23 | 山东省环境保护科学研究设计院有限公司 | Method for detecting bactericide in solid waste |
| CN114910588A (en) * | 2022-05-13 | 2022-08-16 | 厦门泓益检测有限公司 | Synchronous detection method for dalapon, dicamba, pentol, acantol and toxigenin in tea |
| CN114910588B (en) * | 2022-05-13 | 2023-10-10 | 厦门泓益检测有限公司 | Synchronous detection method for couchgrass, dicamba, penta-nitrophenol, fenpyroxim and penconazole in tea |
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Application publication date: 20180612 |