CN105116069A - Reagent and method for rapidly testing pesticide residues - Google Patents
Reagent and method for rapidly testing pesticide residues Download PDFInfo
- Publication number
- CN105116069A CN105116069A CN201510524604.0A CN201510524604A CN105116069A CN 105116069 A CN105116069 A CN 105116069A CN 201510524604 A CN201510524604 A CN 201510524604A CN 105116069 A CN105116069 A CN 105116069A
- Authority
- CN
- China
- Prior art keywords
- reagent
- ethyl acetate
- jolting
- minutes
- pesticide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a reagent for rapidly testing pesticide residues. The reagent comprises a reagent body A and a reagent body B, wherein the reagent body A comprises acetone and ethyl acetate, and the reagent body B is a sodium sulfate aqueous solution. The invention further provides a method for rapidly testing the pesticide residues. The reagent is used in the method. The method includes the steps of 1, placing a to-be-tested sample into a centrifuge tube; 2, adding the reagent body A, and carrying out shaking; 3, adding the reagent body B, and carrying out shaking; 4, carrying out standing or centrifuging, sucking supernatant liquor, and carrying out GC-FPD analysis. According to the reagent and method, the advantages and the disadvantages of an enzymatic inhibition method and a chromatography method are considered, the accuracy of the chromatography method is achieved, and the advantages, including rapidness, convenience and low cost, of the enzymatic inhibition method are achieved. The reagent and method are particularly suitable for large-mass pesticide residue screening and analyzing and particularly suitable for pesticide residue testing laboratories of enterprise and primary-level pesticide testing centers.
Description
Technical field
The present invention relates to detection field, especially for Detecting Pesticide field, particularly, relate to a kind of reagent and method of Fast Determination of Pesticide Residue.
Background technology
China's present stage, be widely used in the detection method of the residues of pesticides of vegetable and fruit, have two classes, a class is inhibiting AChE, and this is a kind of fast detection method; Another kind of is instrument detection method, and comprise and use gas chromatography or liquid chromatography to analyze, its standard has: GB/T5009.20, NY/T761, GB/T20769, and instrument comprises GC-ECD, GC-FPD, GC-MS/MS, LC-MS/MS.
At present, existing fast detection method, for the high-toxic organic phosphorus and the amido formate pesticide residue that detect high concentration, prevents the generation aspect of pesticide poisoning, has played certain effect.But after forbidding production 5 class high-toxic organic phosphorus agricultural chemicals from country, the effect that this method plays is just not obvious.Reason comprises: one, the agricultural chemicals of a lot of classification, and as pyrethrin pesticide, the method can not detect; Its two, even if detect the residual of organophosphorus and amidocarbonic acid ester pesticides, the method can not determine the specific chemical composition detecting agricultural chemicals, certainly can not calculate the persticide residue of sample, cannot judge whether residues of pesticides exceed standard according to regulation GB2763; 3rd, for most of agricultural chemicals, the sensitivity of the method or not high enough.Therefore, the method cannot be monitored, examination goes out the residual vegetables that exceed standard of most agriculture and fruit.
And relatively, the method for stratographic analysis is exactly a kind of classical pesticide residue analysis method, the method can quantitative and qualitative analysis exactly, but it is only suitable for the higher laboratory of technical merit at present, is suitable for arbitration inspection.But because its testing cost is higher, analysis time is longer, the limited amount of each test in laboratory.And due to higher to the technical requirement of personnel, be difficult to the Nong Can testing laboratory spreading to agribusiness and basic unit Nong Jian center.
In " 12 " period, the Ministry of Agriculture in the agricultural sector that major part is at county level, is equipped with GC-ECD, GC-FPD, and some enterprise is also equipped with these equipment.But most of laboratory, can not play device and act on normally, detection method is a bottleneck.
Summary of the invention
For present case, the present invention has compromised the relative merits of above-mentioned two class methods, and both accuracy of possessing of the method for chromatographic, possess again the advantage of the quick, convenient of inhibiting AChE and low cost.The reagent of Fast Determination of Pesticide Residue provided by the present invention and method, compare with the method for traditional stratographic analysis, although more inferior, quicker, convenient and low cost is wanted in accuracy and sensitivity; And compare with inhibiting AChE, although cost is higher, its problem-solving ability is much better than, and its qualitative, quantitative ability is that inhibiting AChE is incomparable.The present invention is specially adapted to the residual Screening analysis of large batch of agriculture, is especially particularly suitable for the Detecting Pesticide laboratory at enterprise, basic unit Nong Jian center.In fact, the reagent of current this Fast Determination of Pesticide Residue and method have been applied in the Nong Can testing laboratory of some and have have received good effect.
On the one hand, theme of the present invention is a kind of reagent of Fast Determination of Pesticide Residue, it is characterized in that, described reagent comprises:
Reagent A: acetoneand ethyl acetate;
Wherein, acetone, acetone, chemical formula: CH3COCH3, CAS accession number 67-64-1, structural formula
ethyl acetate, ethylacetate, chemical formula: C4H8O2, CAS accession number 141-78-6, structural formula
Reagent B: aqueous sodium persulfate solution;
Wherein, sodium sulphate, Sodiumsulfate, chemical formula: Na2SO4, CAS accession number 7757-82-6.
Wherein, as required, described acetoneand ethyl acetate can with arbitrarily than being mixed to get reagent A, and more preferably, the volume ratio of acetoneand ethyl acetate is (1 ~ 5): (5 ~ 1).
As required, described aqueous sodium persulfate solution can be any mass concentration percentage within solubleness, is preferably 5%-10%.
Second aspect, theme of the present invention is a kind of method of Fast Determination of Pesticide Residue, it is characterized in that, uses reagent as claimed in claim 1, comprising:
Step 1: testing sample is placed in centrifuge tube;
Step 2: add reagent A, jolting;
Step 3: add reagent B, jolting;
Step 4: standing or centrifugal, Aspirate supernatant, carries out instrumental analysis.
In a preferred embodiment of the invention, described testing sample is according to the sample of relevant criterion through preparation in early stage.
Described testing sample gets 1 ~ 10g, is preferably 5g.
The jolting time in described step 2 and 3 is 1 ~ 10 minute, is more preferably 2 ~ 3 minutes.
Described leaving standstill is preferably 10 ~ 30 minutes, is more preferably 15 minutes; Centrifugal preferably 2 ~ 8 minutes, be more preferably 4 minutes.
The present invention adopts mixed solvent to extract object, then adds specific salt solusion, makes organic phase and aqueous phase separation, aqueous phase discarded, thus reach the effect of purification.Organic phase is used for stratographic analysis.Can detection organophosphorus pesticide fast.And by further purification, can pyrethrin pesticide be detected, and use the various agricultural chemicals of Mass Spectrometer Method.Key of the present invention is the mixed solvent (acetoneand ethyl acetate) for extracting, and coordinates the salt solusion for purifying, and makes the residual detection of agriculture can complete all operation stepss in a centrifuge tube.Compare with GB/T5009.20, NY/T761, GB/T20769 method, decrease operation steps, decrease the usage quantity of glassware and electric equipment, more more convenient than the method for the current QuECHeRS based on AOAC, step is less, and cost is lower.Be specially adapted to fast, batch quantitative analysis, low to the technical requirement of testing staff, low required by field experiment, reagent cost controls within 20 yuan, each sample (government procurement budget).
The present invention is intended to replace the residual Fast Detection Technique of existing vegetables agriculture (inhibiting AChE), and the residual Fast Detection Technique of vegetables agriculture of China is stepped to a new level, for the food security of China plays a significant role.At present, the remarkable in economical benefits of technique scheme provided by the invention, for the testing agency of this Technique Popularizing to county's one-level, calculate (conservative estimation) with 1000 counties, suppose that 10,000 samples (conservative estimation) are detected in each county every year, the profit of 5 ~ 10 yuan, each sample, can produce the economic benefit of 0.5 ~ 100,000,000 yuan for 1 year.Relative Detecting Pesticide laboratory, its human and material resources saved and financial resources are considerable.
Embodiment
This reagent providing a kind of Fast Determination of Pesticide Residue, it is characterized in that, described reagent comprises:
Reagent A: acetoneand ethyl acetate;
Wherein, acetone, acetone, chemical formula: CH3COCH3, CAS accession number 67-64-1, structural formula
ethyl acetate, ethylacetate, chemical formula: C4H8O2, CAS accession number 141-78-6, structural formula
Reagent B: aqueous sodium persulfate solution;
Wherein, sodium sulphate, Sodiumsulfate, chemical formula: Na2SO4, CAS accession number 7757-82-6.
Wherein, as required, described acetoneand ethyl acetate can with arbitrarily than being mixed to get reagent A, and more preferably, the volume ratio of acetoneand ethyl acetate is (1 ~ 5): (5 ~ 1).
As required, described aqueous sodium persulfate solution can be any mass concentration percentage within solubleness, is preferably 5%-10%.
Present invention also offers a kind of method of Fast Determination of Pesticide Residue, it is characterized in that, use reagent as claimed in claim 1, comprising:
Step 1: testing sample is placed in centrifuge tube;
Step 2: add reagent A, jolting;
Step 3: add reagent B, jolting;
Step 4: standing or centrifugal, Aspirate supernatant, carries out instrumental analysis.
In a preferred embodiment of the invention, described testing sample is preferably according to the sample of relevant criterion through preparation in early stage, as: vegetable and fruit need remove dust and non-edible part.
Described testing sample gets 1 ~ 10g, is preferably 5g.
Preferably, the jolting time in described step 2 and 3 is 1 ~ 10 minute, is more preferably 2 ~ 3 minutes.
Described leaving standstill is preferably 10 ~ 30 minutes, is more preferably 15 minutes; Centrifugal preferably 2 ~ 8 minutes, be more preferably 4 minutes.
By following examples, technical scheme of the present invention is further explained and is illustrated.
Embodiment 1
1, the reagent of Fast Determination of Pesticide Residue
Reagent A: acetoneand ethyl acetate (volume ratio is 1:1);
Reagent B: aqueous sodium persulfate solution (mass concentration percentage: 5%).
2, the method for Fast Determination of Pesticide Residue
Step 1: 5g testing sample is placed in centrifuge tube;
Step 2: add reagent A, jolting 2 minutes;
Step 3: add reagent B, jolting 3 minutes;
Step 4: leave standstill 15 minutes, Aspirate supernatant, carries out GC-FPD analysis.
Embodiment 2
1, the reagent of Fast Determination of Pesticide Residue
Reagent A: acetoneand ethyl acetate (volume ratio is 1.5:1);
Reagent B: aqueous sodium persulfate solution (mass concentration percentage: 10%).
2, the method for Fast Determination of Pesticide Residue
Step 1: 8g testing sample is placed in centrifuge tube;
Step 2: add reagent A, jolting 2 minutes;
Step 3: add reagent B, jolting 3 minutes;
Step 4: centrifugal 4 minutes, Aspirate supernatant, carries out GC-FPD analysis.
Embodiment 3
1, the reagent of Fast Determination of Pesticide Residue
Reagent A: acetoneand ethyl acetate (volume ratio is 1:2);
Reagent B: aqueous sodium persulfate solution (mass concentration percentage: 5%).
2, the method for Fast Determination of Pesticide Residue
Step 1: 1g testing sample is placed in centrifuge tube;
Step 2: add reagent A, jolting 3 minutes;
Step 3: add reagent B, jolting 3 minutes;
Step 4: centrifugal 5 minutes;
Step 5: Aspirate supernatant, dries up;
Step 6, adds mobile phase, carries out LC-MSMS analysis after crossing 0.22um filter membrane.。
Comparative example 4
1, the reagent of Fast Determination of Pesticide Residue
Reagent A: acetoneand ethyl acetate (volume ratio is 1:1);
Reagent B: aqueous sodium persulfate solution (mass concentration percentage: 5%).
2, the method for Fast Determination of Pesticide Residue
Step 1: 2g testing sample is placed in centrifuge tube;
Step 2: add reagent A, jolting 2 minutes;
Step 3: add reagent B, jolting 3 minutes;
Step 4: leave standstill 15 minutes, Aspirate supernatant: in another centrifuge tube, adds the potpourri mixing of PSA and magnesium sulfate;
Step 5: centrifugal 5 minutes, get supernatant, carries out GC-ECD analysis or GC-MS analyzes.
Introduce by embodiment 1-3 and comparative example 4 pre-treating method using GC-FPD, GC-ECD, GC-MS and LC-MSMS to detect residues of pesticides, these methods cover the residue detection of the agricultural compound of the overwhelming majority.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (9)
1. a reagent for Fast Determination of Pesticide Residue, is characterized in that, described reagent comprises:
Reagent A: acetoneand ethyl acetate;
Wherein, acetone, acetone, chemical formula: CH3COCH3, CAS accession number 67-64-1, structural formula
ethyl acetate, ethylacetate, chemical formula: C4H8O2, CAS accession number 141-78-6, structural formula
Reagent B: aqueous sodium persulfate solution;
Wherein, sodium sulphate, Sodiumsulfate, chemical formula: Na2SO4, CAS accession number 7757-82-6.
2. reagent according to claim 1, it is characterized in that, the volume ratio of described acetoneand ethyl acetate is (1 ~ 5): (5 ~ 1).
3. reagent according to claim 1, it is characterized in that, the mass concentration percentage of described aqueous sodium persulfate solution is 5%-10%.
4. a method for Fast Determination of Pesticide Residue, is characterized in that, uses reagent as claimed in claim 1, comprising:
Step 1: testing sample is placed in centrifuge tube;
Step 2: add reagent A, jolting;
Step 3: add reagent B, jolting;
Step 4: standing or centrifugal, Aspirate supernatant, carries out instrumental analysis.
5. method according to claim 4, is characterized in that, described testing sample is according to the sample of relevant criterion through preparation in early stage, comprises vegetable and fruit and need remove dust and non-edible part.
6. method according to claim 4, it is characterized in that, described testing sample gets 1 ~ 10g.
7. method according to claim 4, it is characterized in that, the jolting time in described step 2 and 3 is 1 ~ 10 minute.
8. method according to claim 4, it is characterized in that, described time of repose is 10 ~ 30 minutes.
9. method according to claim 4, it is characterized in that, described centrifugation time is 2 ~ 8 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510524604.0A CN105116069A (en) | 2015-08-24 | 2015-08-24 | Reagent and method for rapidly testing pesticide residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510524604.0A CN105116069A (en) | 2015-08-24 | 2015-08-24 | Reagent and method for rapidly testing pesticide residues |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105116069A true CN105116069A (en) | 2015-12-02 |
Family
ID=54664109
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510524604.0A Pending CN105116069A (en) | 2015-08-24 | 2015-08-24 | Reagent and method for rapidly testing pesticide residues |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105116069A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110361478A (en) * | 2019-08-13 | 2019-10-22 | 深圳市深大检测有限公司 | The detection method of remains of pesticide in a kind of vegetable and fruit |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546988A (en) * | 2003-12-02 | 2004-11-17 | 厦门大学 | Rapid determination method for organophosphorus pesticide residue in vegetable and fruit |
| JP2013164382A (en) * | 2012-02-13 | 2013-08-22 | Shimadzu Corp | Additive agent of matrix for mass analysis |
| CN104181244A (en) * | 2014-08-19 | 2014-12-03 | 广东出入境检验检疫局检验检疫技术中心 | Method for measuring residual quantity of organic chloride pesticides in traditional Chinese medicinal materials |
| CN104374849A (en) * | 2014-11-20 | 2015-02-25 | 沈阳大学 | Method for treating pyrethroid pesticide residue soil environment sample before measurement |
-
2015
- 2015-08-24 CN CN201510524604.0A patent/CN105116069A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546988A (en) * | 2003-12-02 | 2004-11-17 | 厦门大学 | Rapid determination method for organophosphorus pesticide residue in vegetable and fruit |
| JP2013164382A (en) * | 2012-02-13 | 2013-08-22 | Shimadzu Corp | Additive agent of matrix for mass analysis |
| CN104181244A (en) * | 2014-08-19 | 2014-12-03 | 广东出入境检验检疫局检验检疫技术中心 | Method for measuring residual quantity of organic chloride pesticides in traditional Chinese medicinal materials |
| CN104374849A (en) * | 2014-11-20 | 2015-02-25 | 沈阳大学 | Method for treating pyrethroid pesticide residue soil environment sample before measurement |
Non-Patent Citations (7)
| Title |
|---|
| DIPAKSHI SHARMA 等: "Analytical methods for estimation of organophosphorus pesticide residues in fruits and vegetables: A review", 《TALANTA》 * |
| ZHIQIANG HUANG 等: "Simultaneous determination of 102 pesticide residues in Chinese teas by gas chromatography–mass spectrometry", 《JOURNAL OF CHROMATOGRAPHY B》 * |
| 侯如燕 等: "茶鲜叶中拟除虫菊酯类农药残留的检测方法", 《食品与发酵工业》 * |
| 刘明洋 等: "葡萄和土壤中霜脲氰的残留分析方法", 《湖南农业大学学报（自然科学版）》 * |
| 郑永权 等: "蔬菜中拟除虫菊酯类杀虫剂多残留气相色谱检测方法", 《色谱》 * |
| 郭建辉 等: "蔬菜中克螨特残留量的气相色谱法测定", 《福建农业学报》 * |
| 陈九星 等: "溴虫腈在甘蓝及土壤中的残留检测及降解动态", 《环境科学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110361478A (en) * | 2019-08-13 | 2019-10-22 | 深圳市深大检测有限公司 | The detection method of remains of pesticide in a kind of vegetable and fruit |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Whelton et al. | A call for caution in the analysis of lipids and other small biomolecules from archaeological contexts | |
| Fängström et al. | Temporal trends of polybrominated diphenyl ethers and hexabromocyclododecane in milk from Stockholm mothers, 1980–2004 | |
| CN104316634B (en) | The measuring method of volatile organic acids in a kind of cigarette mainstream flue gas | |
| CN112903884A (en) | Method for simultaneously detecting phthalate compounds and metabolites thereof and application thereof | |
| Harvey et al. | Characterization of diesel fuel by chemical separation combined with capillary gas chromatography (GC) isotope ratio mass spectrometry (IRMS) | |
| JP6665629B2 (en) | Method for quantifying components in rubber composition | |
| CN102288691A (en) | Method for assaying short-chain chlorinated paraffin wax in plastics, rubbers and textile materials | |
| CN104458988B (en) | The assay method of one group of biomarker | |
| KR20160143804A (en) | Method for evaluating state of differentiation of cells | |
| Zhang et al. | Levels and congener profiles of polybrominated diphenyl ethers (PBDEs) in primipara breast milk from Shenzhen and exposure risk for breast-fed infants | |
| Su et al. | Using ambient mass spectrometry to explore the origins of phthalate contamination in a mass spectrometry laboratory | |
| Hsu et al. | Background levels of persistent organic pollutants in humans from Taiwan: perfluorooctane sulfonate and perfluorooctanoic acid | |
| CN103308641A (en) | High performance liquid chromatography-tandem mass spectrometry measuring method of three amide herbicides in tobacco and tobacco products | |
| CN103645272B (en) | Method for detecting high-boiling-point substances in industrial products | |
| Zhang et al. | Determination of 123 polycyclic aromatic hydrocarbons and their derivatives in atmospheric samples | |
| CN113189253A (en) | Method for detecting nanoscale plastic particles in soil environment | |
| CN108469485A (en) | Semi-volatile organic matter quickly detects screening method in a kind of new solid waste | |
| CN106596773A (en) | Method for simultaneous and rapidly screening and testing multiple veterinary drug residues in animal-derived food | |
| CN105116069A (en) | Reagent and method for rapidly testing pesticide residues | |
| Morioka et al. | The quantification of the airborne plastic particles of 0.43–11 μm: Procedure development and application to atmospheric environment | |
| CN103926352B (en) | Extraction standard correction-gas chromatography-mass spectrography the assay method of 12 kinds of phthalic esters in a kind of hot melt adhesive | |
| Perrault et al. | Characterization of hafting adhesives using comprehensive two‐dimensional gas chromatography coupled to time‐of‐flight mass spectrometry | |
| CN103926363B (en) | Gas chromatography/mass spectrometry (GC/MS) method for detecting dimethyl fumarate in food additive | |
| Yao et al. | Classification of marine diatoms using pigment ratio suites | |
| CN106802298A (en) | A kind of colorimetric recognition methods of uranyl ion |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151202 |