CN106596829A - Thin-layer chromatography detection method for high-toxic pesticide carbofuran residues - Google Patents
Thin-layer chromatography detection method for high-toxic pesticide carbofuran residues Download PDFInfo
- Publication number
- CN106596829A CN106596829A CN201510658058.XA CN201510658058A CN106596829A CN 106596829 A CN106596829 A CN 106596829A CN 201510658058 A CN201510658058 A CN 201510658058A CN 106596829 A CN106596829 A CN 106596829A
- Authority
- CN
- China
- Prior art keywords
- thin
- detection method
- furadan
- methanol
- chromatography detection
- 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
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses a thin-layer chromatography detection method for high-toxic pesticide carbofuran residues. The method comprises the following steps: a, preparing a test solution; b, preparing a reference solution; c, applying samples of the test solution and the reference solution of carbofuran to the same silica gel plate respectively, developing the samples with a chloroform-ethyl acetate-methanol-water lower solution as a developer, taking out and airing the silica gel plate, and heating the sample at 105 DEG C with a 2% vanillin-sulfuric acid solution as a color developer until spots develop clearly; d, inspecting the silica gel plate after development. The thin-layer chromatography detection method for the high-toxic pesticide carbofuran residues has accurate and reliable detection result, has the advantages of adopting a few procedures, being simple and convenient to operate, short in detection time, low in cost and the like and is quite applicable to industry.
Description
Technical field
The present invention relates to a kind of thin-layered chromatography detection method of high-toxic pesticide Furadan residual.
Background technology
Thin layer chromatography (method) is a kind of conventional detection method, has the advantages that equipment is simple, easy to operate, separating rate is fast, sensitivity and resolution are higher.
Furadan is a kind ofCarbamateClassInsecticideWithNematicide.Formulated by the U.S. within 1963, promoted within 1967.Sterling is whiteCrystallization, dissolubility is 700ppm in water when 25 DEG C, more stable under neutral and acid condition, unstable in alkaline medium, hydrolysis rate withpH ValueAccelerate with the rising of temperature.By Chinese pesticide toxicity grading criteria, Furadan high-toxic pesticide, it is impossible on fruit and vegetables.Furadan is maximum to birds hazardness, as long as bird is looked for food, a Furadan may be fatal.It is poisoned lethal bird or other insecticides by furan, after being looked for food by bird of prey, Small Mammals or reptile, secondary poisoning can be caused and lethal.
Another environmental behaviour feature of Furadan is its residual period in soil longer (degradation half life is 1～2 month), the travelling performance in soil larger (water solubility is 700mg/L), easily cause the pollution to subsoil water in the sand soil area that precipitation is big, level of ground water is shallow, be that this U.S. is limited Furadan using some provincialism have been made.Hazard property：Meet naked light, hyperpyrexia is flammable.Decomposes release poisonous nitrogen oxide flue gas.
In prior art, Furadan is generally detected using high performance liquid chromatography (HPLC), liquid chromatography/mass spectrometry combination analysis method (LC/MS), gas chromatography/mass spectrometry analytic process (GC/MS), fluorescence probe method, but conventional physico-chemical analysis method needs the conditions such as expensive instrument and equipment, skilled practitioner, and operating process is complicated, detection time is longer, therefore limit its range of application, it is difficult to the popularization and application in produce reality.
Accordingly, it would be desirable to inventing, a kind of operation is few, detection easy to operate new method.
The content of the invention
It is an object of the invention to provide a kind of thin-layered chromatography detection method of high-toxic pesticide Furadan residual.
A kind of thin-layered chromatography detection method of high-toxic pesticide Furadan residual that the present invention is provided, comprises the following steps:
A, prepare need testing solution:Furadan is taken, adds methanol A, supersound process to filter, take supernatant;Supernatant is filtered with microporous filter membrane, is evaporated, and after residue is with 10% v/v ammonia solvents, is extracted with water-saturated n-butanol, obtains extract;Extract is evaporated, residue methanol B dissolves, and obtains final product need testing solution;
B, preparation reference substance solution:The dissolving of Furadan methanol is taken, the reference substance solution of Furadan is obtained.
C, by need testing solution, the reference substance solution of Furadan, respectively, in same silica gel plate, the lower floor's solution with one acetic acid ethyl ester of chloroform-Methanol-water is as developing solvent for point sample, launch, take out, dry, with 2% vanillin-sulfuric acid solution as developer, 105 DEG C to be heated to spot development clear;
D, the silica gel plate inspected after colour developing, you can.
Further, in step a, the high-toxic pesticide is Furadan.
Further, in step a, the Chinese medicine composition is prepared from according to following steps:
1., fetch earth earth, is crushed to 80 mesh, drying, respectively obtains soil coarse powder
2., under the conditions of -10 DEG C ~ -20 DEG C, the soil coarse powder that 1. step is obtained further is crushed to the granularity of 100 mesh ~ 800 mesh, obtains soil superfine powder;
3., by soil superfine powder, 80 mesh sieves are crossed in granulation, drying, are obtained final product.
Further, in step a, Furadan is 1 with the w/v of methanol A:15g/ml;Methanol A, 10% v/v ammonia, water-saturated n-butanol, the volume ratio of methanol B are 6:2:3:1.
Further, in step a, the time of supersound process is 60min;The aperture of microporous filter membrane is 0.45 μm.
Further, in step b, the reference substance solution concentration of Furadan is 1mg/ml.
Further, in step c, the silica gel plate is silica gel g thin-layer plate.
Further, in step C, in chloroform-acetic acid ethyl ester-methanol-water, chloroform, acetic acid ethyl ester, methanol, the volume ratio of water are 20:40:22:1.
Further, in step d, the silica gel plate after colour developing, on position corresponding with reference substance chromatograph, the speckle of test sample Chromatogram display same color.
The thin-layered chromatography detection method of high-toxic pesticide Furadan residual of the present invention, can be detected with high-toxic pesticide Furadan, testing result is accurate, reliable, while, the inventive method has that operation is few, easy to operate, detection time is short, low cost and other advantages, the application being especially suitable in industry.
Obviously, the above of the invention, according to the glycosides of this area technological know-how and customary means are led to, and under the premise of without departing from above-mentioned basic fundamental thought of the invention, can also be made the modification of other various ways, be replaced or change.
By the following examples the specific embodiment of form, is described in further detail again to the above of the present invention.But this scope for being interpreted as above-mentioned theme of the invention should not be only limitted to Examples below.All technologies realized based on the above of the present invention belong to the scope of the present invention.
Description of the drawings
Fig. 1 is the thin layer chromatography testing result of Furadan of the present invention.
Specific embodiment
Raw material, equipment used in the specific embodiment of the invention is known product, is obtained by buying commercially available prod.
The thin-layered chromatography detection method of embodiment 1, Chinese medicine composition of the present invention
1st, Furadan is prepared
Soil is crushed to into 80 mesh using Universalpulverizer, is dried, make the moisture Control of soil coarse powder 6% ~ 8%;Under the conditions of temperature is for -10 DEG C ~ -20 DEG C, post-drying of pelletizing crosses 80 mesh sieves.
2nd, detection method
By the grinding of above-mentioned soil particle, precision weighs powder 2.0g, in being placed in triangular flask, plus methanol 30m1, supersound process 60min, filter, take supernatant;Supernatant is filtered with 0.45 μm of microporous filter membrane (PTFE), is placed in evaporating dish and is evaporated;Residue 10ml 10% (V/V) ammonia solvent, places l0min, shakes frequently;Solution is moved in separatory funnel, is extracted 3 times with 15m1 water-saturated n-butanols;Combining extraction liquid, is evaporated with evaporating dish, and residue adds 5m1 methanol to dissolve, and obtains final product need testing solution;
Furadan is taken, methanol is added, solution of every 1ml containing 1mg is respectively prepared, as reference substance solution.
Test according to thin layer chromatography (2010 editions annex VI B of Pharmacopoeia of People's Republic of China), draw above-mentioned need testing solution, each 3 μ 1 of reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetic acid ethyl ester-methanol-water (20:40:22:1) lower floor's solution is developing solvent, is launched, and is taken out, and is dried, and is sprayed with 2% vanillin-sulfuric acid solution, is heated to spot development at 105 DEG C clear;Its testing result is shown in Fig. 1, on position corresponding with reference substance chromatograph, the speckle of test sample Chromatogram display same color.
The thin-layered chromatography detection method of high-toxic pesticide Furadan residual of the present invention, high-toxic pesticide Furadan can be detected, testing result is accurate, reliable, while, the inventive method has that operation is few, easy to operate, detection time is short, low cost and other advantages, the application being especially suitable in industry.
Claims (9)
1. the thin-layered chromatography detection method that a kind of high-toxic pesticide Furadan is remained, it is characterised in that:The discrimination method is comprised the following steps:
A, prepare need testing solution:Furadan is taken, adds methanol A, supersound process to filter, take supernatant;Supernatant is filtered with microporous filter membrane, is evaporated, and after residue is with 10% v/v ammonia solvents, is extracted with water-saturated n-butanol, obtains extract;Extract is evaporated, residue methanol B dissolves, and obtains final product need testing solution；
B, preparation reference substance solution:The dissolving of Furadan methanol is taken, the reference substance solution of Furadan is obtained；
C, by need testing solution, the reference substance solution of Furadan, respectively point sample is in same silica gel plate, lower floor's solution with chloroform-acetic acid ethyl ester-methanol-water is as developing solvent, launch, take out, dry, with 2% vanillin-sulfuric acid solution as developer, 105 DEG C are heated to spot development clearly, the silica gel plate after being developed the color；
D, the silica gel plate inspected after colour developing, you can.
2. thin-layered chromatography detection method according to claim 1, it is characterised in that：In step a, the high-toxic pesticide is Furadan.
3. thin-layered chromatography detection method according to claim 2, it is characterised in that：In step a, the Furadan thing is prepared from according to following steps：
1., fetch earth earth, is crushed to 80 mesh, drying, respectively obtains soil coarse powder；
2., under the conditions of -10 DEG C ~ -20 DEG C, the soil coarse powder that 1. step is obtained further is crushed to the granularity of 100 mesh ~ 800 mesh, obtains soil superfine powder；
3., by soil superfine powder, 80 mesh sieves are crossed in granulation, drying, are obtained final product.
4. thin-layered chromatography detection method according to claim 1, it is characterised in that：In step a, Furadan is 1 with the w/v of methanol A:15g/ml；Methanol A, 10% v/v ammonia, water-saturated n-butanol, the volume ratio of methanol B are 6:2:3:1.
5. thin-layered chromatography detection method according to claim 1, it is characterised in that：In step a, the time of supersound process is 60min；The aperture of microporous filter membrane is 0.45 μm.
6. thin-layered chromatography detection method according to claim 1, it is characterised in that：In step b, the concentration of the reference substance solution of Furadan is 1mg/ml.
7. thin-layered chromatography detection method according to claim 1, it is characterised in that：In step c, the silica gel plate is silica gel g thin-layer plate.
8. thin-layered chromatography detection method according to claim 1, it is characterised in that：In step c, in chloroform-acetic acid ethyl ester-methanol-water, chloroform, acetic acid ethyl ester, methanol, the volume ratio of water are 20:40:22:l.
9. thin-layered chromatography detection method according to claim 1, it is characterised in that：In step d, the silica gel plate after colour developing, on position corresponding with reference substance chromatograph, the speckle of test sample Chromatogram display same color.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510658058.XA CN106596829A (en) | 2015-10-14 | 2015-10-14 | Thin-layer chromatography detection method for high-toxic pesticide carbofuran residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510658058.XA CN106596829A (en) | 2015-10-14 | 2015-10-14 | Thin-layer chromatography detection method for high-toxic pesticide carbofuran residues |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106596829A true CN106596829A (en) | 2017-04-26 |
Family
ID=58551773
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510658058.XA Pending CN106596829A (en) | 2015-10-14 | 2015-10-14 | Thin-layer chromatography detection method for high-toxic pesticide carbofuran residues |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106596829A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109752480A (en) * | 2017-11-05 | 2019-05-14 | 江苏维赛科技生物发展有限公司 | A kind of remaining thin-layered chromatography detection method of high poison antistaling agent o-phenyl phenol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558330A (en) * | 2013-10-08 | 2014-02-05 | 九芝堂股份有限公司 | Thin-layer identification chromatography method of stomach-strengthening ulcer-curing preparation |
| CN104865341A (en) * | 2015-06-05 | 2015-08-26 | 成都乾坤动物药业有限公司 | Thin-layer chromatography detection method of traditional Chinese medicine composition for increasing animal immunity |
| CN104931640A (en) * | 2015-06-05 | 2015-09-23 | 成都乾坤动物药业有限公司 | Thin layer chromatographic detection method for traditional Chinese medicine composition for improving immunity of animals |
-
2015
- 2015-10-14 CN CN201510658058.XA patent/CN106596829A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103558330A (en) * | 2013-10-08 | 2014-02-05 | 九芝堂股份有限公司 | Thin-layer identification chromatography method of stomach-strengthening ulcer-curing preparation |
| CN104865341A (en) * | 2015-06-05 | 2015-08-26 | 成都乾坤动物药业有限公司 | Thin-layer chromatography detection method of traditional Chinese medicine composition for increasing animal immunity |
| CN104931640A (en) * | 2015-06-05 | 2015-09-23 | 成都乾坤动物药业有限公司 | Thin layer chromatographic detection method for traditional Chinese medicine composition for improving immunity of animals |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109752480A (en) * | 2017-11-05 | 2019-05-14 | 江苏维赛科技生物发展有限公司 | A kind of remaining thin-layered chromatography detection method of high poison antistaling agent o-phenyl phenol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Oellig et al. | Planar solid phase extraction clean-up for pesticide residue analysis in tea by liquid chromatography–mass spectrometry | |
| Pirard et al. | Development and validation of a multi-residue method for pesticide determination in honey using on-column liquid–liquid extraction and liquid chromatography–tandem mass spectrometry | |
| Zuin et al. | Stir bar sorptive extraction and high-performance liquid chromatography–fluorescence detection for the determination of polycyclic aromatic hydrocarbons in Mate teas | |
| Sadowska-Rociek et al. | Application of QuEChERS method for simultaneous determination of pesticide residues and PAHs in fresh herbs | |
| Alcaide-Molina et al. | High through-put aflatoxin determination in plant material by automated solid-phase extraction on-line coupled to laser-induced fluorescence screening and determination by liquid chromatography–triple quadrupole mass spectrometry | |
| JP2007155657A (en) | Method for analyzing agricultural chemicals using liquid chromatography-tandem mass spectrometry (lc-ms/ms) | |
| De Zeeuw et al. | Δ1-Tetrahydrocannabinolic acid, an important component in the evaluation of cannabis products | |
| Das | Recent developments in clean up techniques of pesticide residue analysis for toxicology study: a critical review | |
| Haraguchi et al. | Simultaneous determination of trace pesticides in urban air | |
| CN104374849A (en) | Method for treating pyrethroid pesticide residue soil environment sample before measurement | |
| Khan | Determination of diquat and paraquat residues in soil by gas chromatography | |
| Sun et al. | Stability studies of propoxur herbicide in environmental water samples by liquid chromatography–atmospheric pressure chemical ionization ion-trap mass spectrometry | |
| Zuo et al. | Application of dispersive liquid–liquid microextraction based on solidification of floating organic droplet Multi‐residue method for the simultaneous determination of polychlorinated biphenyls, organochlorine, and pyrethroid pesticides in aqueous sample | |
| CN106596829A (en) | Thin-layer chromatography detection method for high-toxic pesticide carbofuran residues | |
| Yuliani et al. | Effects of particle size, extraction time, and solvent on daidzein yield extracted from tempeh | |
| Borahan et al. | An analytical strategy for propoxur determination in raisin samples with matrix matching method after dispersive liquid-liquid microextraction | |
| Soares et al. | Determination of pesticides in soil using a hyphenated extraction technique | |
| Estevão et al. | Binary solvent dispersive liquid-liquid microextraction for the determination of pesticides in natural water samples | |
| Laturnus et al. | Organic waste products in agriculture‐monitoring the waste constituents phthalate esters in soil‐crop system by gas chromatography and ion trap tandem mass spectrometry | |
| Zhang et al. | Analysis of chlorpyrifos and chlorpyrifos-methyl residues in multi-environmental media by cloud-point extraction and HPLC | |
| CN105628843B (en) | The immobilon-p extraction gas-chromatography electron capture detection method of 8 kinds of pyrethroid pesticides in water body | |
| Chen et al. | Method validation for simultaneous quantification of some high-risk pesticides in surface water samples by SPE-LC-MS/MS | |
| Souza et al. | A reliable and cost-effective method for determination of endocrine-disrupting compounds in coastal waters, suspended particulate matter, and sediments by ultrafast liquid chromatography coupled to photodiode array and fluorescence detectors | |
| Gaynor et al. | Pentafluorobenzyl,(trifluoromethyl) benzyl and diazomethane alkylation of bentazon for residue determination in soil by gas chromatography | |
| Liu et al. | Simultaneous determination of 15 multiresidue organophosphorous pesticides in Camellia oil by MSPD-GC–MS |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170426 |
|
| WD01 | Invention patent application deemed withdrawn after publication |