CN104374849A - Method for treating pyrethroid pesticide residue soil environment sample before measurement - Google Patents
Method for treating pyrethroid pesticide residue soil environment sample before measurement Download PDFInfo
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- CN104374849A CN104374849A CN201410666464.6A CN201410666464A CN104374849A CN 104374849 A CN104374849 A CN 104374849A CN 201410666464 A CN201410666464 A CN 201410666464A CN 104374849 A CN104374849 A CN 104374849A
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Abstract
The invention discloses a method for treating a pyrethroid pesticide residue soil environment sample before measurement, and relates to a method for analyzing and pretreating organic pollutants in soil environment samples. The method comprises the following steps: grinding a soil sample; performing freeze drying on the collected soil environment sample, grinding and crushing; extracting, namely accurately weighing the soil sample, adding petroleum ether/acetone, performing ultrasonic extraction, and adding 2 percent of sodium sulfate aqueous solution into a supernatant; concentrating, namely drying an upper-layer organic phase by virtue of anhydrous sodium sulfate, evaporating and concentrating; purifying by adopting a glass chromatography silica-gel column method, and performing wet column packing; concentrating and making up to the volume, namely dissolving and making up to the volume by using chromatographic n-hexane, and measuring the content of pyrethroid by adopting a gas chromatograph or a gas chromatograph-mass spectrometer. According to the method, multiple pyrethroid pesticide compounds can be extracted from the soil environment samples and are purified; according to the method, the cost is low, reproducibility and stability are high, and methods and technical supports are provided for detection and evaluation of pyrethroid pesticides in the soil environment samples.
Description
Technical field
The present invention relates to a kind of soil environment sample organic pollutant analysis pre-treating method, particularly relate to the disposal route before a kind of pyrethroid pesticide remained soil environment sample determination.
Background technology
Pyrethroid pesticide is chemical constitution according to natural pyrethrum and a class of copying contains the trimethylene Ester of phenoxy group, because of its have efficiently, low toxicity and the feature such as metabolism is rapid, pyrethroid pesticide has obtained using more and more widely since being born from 1973 in crops deinsectization and health pest control.At present, along with part high-toxic organic phosphorus and carbamate chemicals for agriculture forbidding aborning, the use amount of pyrethroid pesticide is only second to organophosphorus insecticide, occupies the 2nd of biocides market.At present, in global range pyrethroid commercial kind to have more than 70, wherein conventional kind comprises decis, cypermethrin, efficient chlorine fluorine hydrocyanic ester, Biphenthrin, cypermethrin, fenvalerate, Tefluthrin and cyfloxylate etc., and they account for 84.6% of the pyrethroid insecticides market share.
But, along with pyrethroid insectide increasingly extensive apply, also bring residues of pesticides and the problem of environmental pollution of agricultural product simultaneously.Pesticide-Polluted Soil has become one of important environmental problem of China.Investigation shows, only fraction pyrethroid pesticide can act on target biology, have 80% even more parts then act on non-target organism and remain the surrounding mediums such as soil.In soil, pyrethroid pesticide is residual, directly causes the pollution of agricultural product, and and then threatens population health by the transmission of food chain.Along with such agricultural chemicals is applied more and more widely, the soil contamination problem caused thus can be increasingly general and serious, therefore, systematically carry out the researchs such as the soil environmental quality standard behavior of pyrethroid pesticide and associated restoration technology as early as possible comprehensively and seem increasingly urgent, and in accurate analysis and assessment soil environment sample, the residual quantity of pyrethroid pesticide becomes the necessary means and technical guarantee of carrying out above-mentioned research.
Soil due to self component complicated, and other organic contaminants are as the residual of the components such as palycyclic aromatic, organochlorine and organophosphorus pesticide and interference, make the extracting and developing of pyrethroid pesticide, the difficulty of purification and enrichment strengthens.At present about amount pyrethroid pesticide remained in soil environment sample detects the report of pre-treating method, there is the problem that in extraction, purification process, the consumption of organic solvent amount is larger.For this reason, the present invention establishes the disposal route before a kind of Pyrethroid pesticides residue soil environment sample determination, the express-analysis that in soil, multiple pyrethroid pesticide is residual can be carried out, for situation pyrethroid pesticide remained in Monitoring and assessing soil provides foundation simultaneously.
Summary of the invention
The object of the present invention is to provide the disposal route before a kind of pyrethroid pesticide remained soil environment sample determination, multiple pyrethroid pesticide compound can extract and purify by the method from soil environment sample, the cost of method is low, reappearance and stability high, be soil environment sample pyrethroid pesticide detecting and assessing supplying method and technical support.
The object of the invention is to be achieved through the following technical solutions:
This method comprises following process:
1, pedotheque is pulverized: by the soil environment sample freeze drying gathered, grind with planetary ball mill, crosses 100 order stainless steel sifts.
2, extract: accurate weighing 5-10 gram pedotheque is in 150 milliliters of tool plug triangular flasks, add 25 milliliters of sherwood oil/acetone (volume ratio 2:1) as extraction agent, shake up immersion after 2 hours, ultrasonic extraction 20 minutes under 100 hertz of conditions, after stratification, supernatant is transferred in 125 milliliters of separating funnels, repeat said extracted process 1 time, supernatant is transferred in separating funnel, adds 2% aqueous sodium persulfate solution 30 milliliters, jolting left standstill 10 minutes after 3 minutes, made organic phase and aqueous phase layering.
3, concentrated: upper organic phase, after 10 grams of anhydrous sodium sulfate dryings, rotates evaporation and concentration to 1 milliliter under 40 DEG C of conditions.
4, purify: adopt the purification of glass chromatography silicagel column method, wet method dress post.At a small amount of absorbent cotton of self-control glass little column bottom pad of high 15 centimetres of diameter 0.8 centimetre, 2 grams, the 100 order silica gel, the 1 gram of anhydrous sodium sulfate powder that load 1 gram of anhydrous sodium sulfate powder successively from bottom to up again, soaked through sherwood oil, rap chromatography glass column tube wall to make to enrich, with the pre-drip washing chromatographic column of 5 sherwood oil, discard pre-leaching liquid, when liquid level has just been exposed on anhydrous sodium sulfate surface, above-mentioned 1 milliliter of concentrated extracting solution is joined in chromatographic column, bottle is concentrated afterwards by 0.5 milliliter of petroleum ether, make it to shift completely, discard efflux.When concentrated extracting solution drops to sodium sulphate surface, upper strata, in chromatographic column, add petrol ether/ethyl acetate (volume ratio is 10:1), and start to collect eluent simultaneously, divide and add 20 milliliters of petrol ether/ethyl acetate mixing leacheates for 4 times altogether.
5, concentrated constant volume: by concentrated for the eluent rotary evaporation after purification near dry under 40 DEG C of conditions, nitrogen dries up, and is settled to 1.0 milliliters with chromatogram n-hexane dissolution, adopts gas chromatograph or gas chromatograph-mass spectrometer (GCMS) to measure the content of pyrethroid.
Advantage of the present invention and effect are:
The method saves organic solvent, cost of determination is low, sample purification is effective, accuracy, stability and reliability are high, can carry out the rapid extraction that in soil, multiple pyrethroid pesticide is residual, be situation supplying method pyrethroid pesticide remained in Monitoring and assessing soil and technical guarantee simultaneously.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
1, pedotheque is pulverized: by the soil environment sample freeze drying gathered, grind with planetary ball mill, crosses 100 order stainless steel sifts.
2, extract: accurate weighing 5 grams of pedotheques are in 150 milliliters of tool plug triangular flasks, add 25 milliliters of sherwood oil/acetone (volume ratio 2:1) as extraction agent, shake up immersion after 2 hours, ultrasonic extraction 20 minutes under 100 hertz of conditions, after stratification, supernatant is transferred in 125 milliliters of separating funnels, repeat said extracted process 1 time, supernatant is transferred in separating funnel, adds 2% aqueous sodium persulfate solution 30 milliliters, jolting left standstill 10 minutes after 3 minutes, made organic phase and aqueous phase layering.
3, concentrated: upper organic phase, after 10 grams of anhydrous sodium sulfate dryings, rotates evaporation and concentration to 1 milliliter under 40 DEG C of conditions.
4, purify: adopt the purification of glass chromatography silicagel column method, wet method dress post.At a small amount of absorbent cotton of self-control glass little column bottom pad of high 15 centimetres of diameter 0.8 centimetre, 2 grams, the 100 order silica gel, the 1 gram of anhydrous sodium sulfate powder that load 1 gram of anhydrous sodium sulfate powder successively from bottom to up again, soaked through sherwood oil, rap chromatography glass column tube wall to make to enrich, with the pre-drip washing chromatographic column of 5 sherwood oil, discard pre-leaching liquid, when liquid level has just been exposed on anhydrous sodium sulfate surface, above-mentioned 1 milliliter of concentrated extracting solution is joined in chromatographic column, bottle is concentrated afterwards by 0.5 milliliter of petroleum ether, make it to shift completely, discard efflux.When concentrated extracting solution drops to sodium sulphate surface, upper strata, in chromatographic column, add petrol ether/ethyl acetate (volume ratio is 10:1), and start to collect eluent simultaneously, divide and add 20 milliliters of petrol ether/ethyl acetate mixing leacheates for 4 times altogether.
5, concentrated constant volume: by concentrated for the eluent rotary evaporation after purification near dry under 40 DEG C of conditions, nitrogen dries up, and is settled to 1.0 milliliters with chromatogram n-hexane dissolution, adopts gas chromatograph or gas chromatograph-mass spectrometer (GCMS) to measure the content of pyrethroid.
Embodiment 2
1, pedotheque is pulverized: by the soil environment sample freeze drying gathered, grind with planetary ball mill, crosses 100 order stainless steel sifts.
2, extract: accurate weighing 8 grams of pedotheques are in 150 milliliters of tool plug triangular flasks, add 25 milliliters of sherwood oil/acetone (volume ratio 2:1) as extraction agent, shake up immersion after 2 hours, ultrasonic extraction 20 minutes under 100 hertz of conditions, after stratification, supernatant is transferred in 125 milliliters of separating funnels, repeat said extracted process 1 time, supernatant is transferred in separating funnel, adds 2% aqueous sodium persulfate solution 30 milliliters, jolting left standstill 10 minutes after 3 minutes, made organic phase and aqueous phase layering.
3, concentrated: upper organic phase, after 10 grams of anhydrous sodium sulfate dryings, rotates evaporation and concentration to 1 milliliter under 40 DEG C of conditions.
4, purify: adopt the purification of glass chromatography silicagel column method, wet method dress post.At a small amount of absorbent cotton of self-control glass little column bottom pad of high 15 centimetres of diameter 0.8 centimetre, 2 grams, the 100 order silica gel, the 1 gram of anhydrous sodium sulfate powder that load 1 gram of anhydrous sodium sulfate powder successively from bottom to up again, soaked through sherwood oil, rap chromatography glass column tube wall to make to enrich, with the pre-drip washing chromatographic column of 5 sherwood oil, discard pre-leaching liquid, when liquid level has just been exposed on anhydrous sodium sulfate surface, above-mentioned 1 milliliter of concentrated extracting solution is joined in chromatographic column, bottle is concentrated afterwards by 0.5 milliliter of petroleum ether, make it to shift completely, discard efflux.When concentrated extracting solution drops to sodium sulphate surface, upper strata, in chromatographic column, add petrol ether/ethyl acetate (volume ratio is 10:1), and start to collect eluent simultaneously, divide and add 20 milliliters of petrol ether/ethyl acetate mixing leacheates for 4 times altogether.
5, concentrated constant volume: by concentrated for the eluent rotary evaporation after purification near dry under 40 DEG C of conditions, nitrogen dries up, and is settled to 1.0 milliliters with chromatogram n-hexane dissolution, adopts gas chromatograph or gas chromatograph-mass spectrometer (GCMS) to measure the content of pyrethroid.
Embodiment 3
1, pedotheque is pulverized: by the soil environment sample freeze drying gathered, grind with planetary ball mill, crosses 100 order stainless steel sifts.
2, extract: accurate weighing 10 grams of pedotheques are in 150 milliliters of tool plug triangular flasks, add 25 milliliters of sherwood oil/acetone (volume ratio 2:1) as extraction agent, shake up immersion after 2 hours, ultrasonic extraction 20 minutes under 100 hertz of conditions, after stratification, supernatant is transferred in 125 milliliters of separating funnels, repeat said extracted process 1 time, supernatant is transferred in separating funnel, adds 2% aqueous sodium persulfate solution 30 milliliters, jolting left standstill 10 minutes after 3 minutes, made organic phase and aqueous phase layering.
3, concentrated: upper organic phase, after 10 grams of anhydrous sodium sulfate dryings, rotates evaporation and concentration to 1 milliliter under 40 DEG C of conditions.
4, purify: adopt the purification of glass chromatography silicagel column method, wet method dress post.At a small amount of absorbent cotton of self-control glass little column bottom pad of high 15 centimetres of diameter 0.8 centimetre, 2 grams, the 100 order silica gel, the 1 gram of anhydrous sodium sulfate powder that load 1 gram of anhydrous sodium sulfate powder successively from bottom to up again, soaked through sherwood oil, rap chromatography glass column tube wall to make to enrich, with the pre-drip washing chromatographic column of 5 sherwood oil, discard pre-leaching liquid, when liquid level has just been exposed on anhydrous sodium sulfate surface, above-mentioned 1 milliliter of concentrated extracting solution is joined in chromatographic column, bottle is concentrated afterwards by 0.5 milliliter of petroleum ether, make it to shift completely, discard efflux.When concentrated extracting solution drops to sodium sulphate surface, upper strata, in chromatographic column, add petrol ether/ethyl acetate (volume ratio is 10:1), and start to collect eluent simultaneously, divide and add 20 milliliters of petrol ether/ethyl acetate mixing leacheates for 4 times altogether.
5, concentrated constant volume: by concentrated for the eluent rotary evaporation after purification near dry under 40 DEG C of conditions, nitrogen dries up, and is settled to 1.0 milliliters with chromatogram n-hexane dissolution, adopts gas chromatograph or gas chromatograph-mass spectrometer (GCMS) to measure the content of pyrethroid.
Claims (2)
1. the disposal route before pyrethroid pesticide remained soil environment sample determination, it is characterized in that, described method comprises following process:
1) pedotheque is pulverized: by the soil environment sample freeze drying gathered, grind, and crosses 100 mesh sieves;
2) extract: accurate weighing pedotheque is in triangular flask, add sherwood oil/acetone as extraction agent, after shaking up immersion, ultrasonic extraction, after stratification, supernatant is repeated said extracted process 1 time, supernatant is added 2% aqueous sodium persulfate solution, leave standstill after jolting, make organic phase and aqueous phase layering;
3) concentrated: upper organic phase, after anhydrous sodium sulfate drying, rotates evaporation and concentration under 40 DEG C of conditions;
4) purify: adopt the purification of glass chromatography silicagel column method, wet method dress post;
5) concentrated constant volume: by concentrated for the eluent rotary evaporation after purification near dry under 40 DEG C of conditions, nitrogen dries up, with chromatogram n-hexane dissolution constant volume, adopts gas chromatograph or gas chromatograph-mass spectrometer (GCMS) to measure the content of pyrethroid.
2. the disposal route before pyrethroid pesticide remained soil environment sample determination according to claim 1, is characterized in that, described wet method dress post; At a small amount of absorbent cotton of self-control glass little column bottom pad of high 15 centimetres of diameter 0.8 centimetre, 2 grams, the 100 order silica gel, the 1 gram of anhydrous sodium sulfate powder that load 1 gram of anhydrous sodium sulfate powder successively from bottom to up again, soaked through sherwood oil, rap chromatography glass column tube wall to make to enrich, with the pre-drip washing chromatographic column of 5 sherwood oil, discard pre-leaching liquid, when liquid level has just been exposed on anhydrous sodium sulfate surface, above-mentioned 1 milliliter of concentrated extracting solution is joined in chromatographic column, bottle is concentrated afterwards by 0.5 milliliter of petroleum ether, make it to shift completely, discard efflux; When concentrated extracting solution drops to sodium sulphate surface, upper strata, in chromatographic column, adding petrol ether/ethyl acetate, (volume ratio is 10:1, and starts to collect eluent simultaneously, divides and adds 20 milliliters of petrol ether/ethyl acetate mixing leacheates for 4 times altogether.
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Cited By (7)
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| CN105116069A (en) * | 2015-08-24 | 2015-12-02 | 上海睿致生物科技有限公司 | Reagent and method for rapidly testing pesticide residues |
| CN105510498A (en) * | 2015-12-22 | 2016-04-20 | 广东贝源检测技术股份有限公司 | GC-MS (gas chromatography-mass spectrometry) method for determining common pesticides in soil |
| CN105645704A (en) * | 2015-12-29 | 2016-06-08 | 安徽理工大学 | Method for treating, extracting and purifying organic chloride pesticide in sediment of coal mining subsidence area |
| CN105891354A (en) * | 2016-03-31 | 2016-08-24 | 山东五洲检测有限公司 | Detection method for content of fenthion in sorghum planting soil |
| CN107389808A (en) * | 2017-06-28 | 2017-11-24 | 防城港市质量技术监督局 | The detection method of vegetable pesticide residue |
| CN113776906A (en) * | 2021-09-07 | 2021-12-10 | 山东省环境保护科学研究设计院有限公司 | Method for improving detection rate of polycyclic aromatic hydrocarbons in high-water-content soil sample |
| US11585790B1 (en) | 2020-07-31 | 2023-02-21 | Pace Analytical Services, LLC | Analytical herbicide detection technology |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105116069A (en) * | 2015-08-24 | 2015-12-02 | 上海睿致生物科技有限公司 | Reagent and method for rapidly testing pesticide residues |
| CN105510498A (en) * | 2015-12-22 | 2016-04-20 | 广东贝源检测技术股份有限公司 | GC-MS (gas chromatography-mass spectrometry) method for determining common pesticides in soil |
| CN105645704A (en) * | 2015-12-29 | 2016-06-08 | 安徽理工大学 | Method for treating, extracting and purifying organic chloride pesticide in sediment of coal mining subsidence area |
| CN105891354A (en) * | 2016-03-31 | 2016-08-24 | 山东五洲检测有限公司 | Detection method for content of fenthion in sorghum planting soil |
| CN105891354B (en) * | 2016-03-31 | 2018-03-09 | 山东五洲检测有限公司 | The detection method of content of fenthion in a kind of sorghum planting soil |
| CN107389808A (en) * | 2017-06-28 | 2017-11-24 | 防城港市质量技术监督局 | The detection method of vegetable pesticide residue |
| US11585790B1 (en) | 2020-07-31 | 2023-02-21 | Pace Analytical Services, LLC | Analytical herbicide detection technology |
| CN113776906A (en) * | 2021-09-07 | 2021-12-10 | 山东省环境保护科学研究设计院有限公司 | Method for improving detection rate of polycyclic aromatic hydrocarbons in high-water-content soil sample |
| CN113776906B (en) * | 2021-09-07 | 2023-01-10 | 山东省环境保护科学研究设计院有限公司 | Method for improving detection rate of polycyclic aromatic hydrocarbons in high-water-content soil sample |
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Application publication date: 20150225 |