Method for detecting residual organic solvents in soil and water by adopting gas chromatography-mass spectrometry method

A gas chromatography and organic solvent technology, used in pesticide adjuvant residue detection, drug detection, and environmental safety fields, can solve the problems of different chemical properties, high promotion costs, large differences in boiling points and polarities, etc., and achieves easy operation and operation. Convenience and increased sensitivity

A gas chromatography and organic solvent technology, used in pesticide adjuvant residue detection, drug detection, and environmental safety fields, can solve the problems of different chemical properties, high promotion costs, large differences in boiling points and polarities, etc., and achieves easy operation and operation. Convenience and increased sensitivity

CN106526018AActive Publication Date: 2017-03-22INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS

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  • Method for detecting residual organic solvents in soil and water by adopting gas chromatography-mass spectrometry method
  • Method for detecting residual organic solvents in soil and water by adopting gas chromatography-mass spectrometry method
  • Method for detecting residual organic solvents in soil and water by adopting gas chromatography-mass spectrometry method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] S11. Instruments and reagents

[0044] 7890A / 5975C gas chromatography-mass spectrometry (Agilent, USA); XS 105 electronic balance (Mettler Toledo, Switzerland); QL-901 vortex mixer (Qilin Bell Instrument Co., Ltd., Haimen City); BiofugeStratos desktop high-speed freezer Centrifuge (Thermo Company, USA).

[0045] Acetonitrile, ethyl acetate, toluene, acetone, DMF, DMSO (chromatographically pure, Merck, Germany); o-xylene, m-xylene, p-xylene (chromatographic standard, Sinopharm Chemical Reagent Beijing Co., Ltd.); Wahaha drinking Purified water (Wahaha Group); other reagents were of analytical grade, purchased from Beijing Baihui Jiaxing Technology Co., Ltd.

[0046] Soil and water samples were collected from farmlands around Yanjiao.

[0047] S12, standard solution preparation

[0048] Acetonitrile, ethyl acetate, and acetone are formulated into an extract with a volume ratio of 1:1.2:1.2;

[0049] Toluene, o-xylene, p-xylene, m-xylene, DMF and DMSO are prepared with...

Embodiment 2

[0064] S21. Instruments and reagents

[0065] Same as S11.

[0066] S22. Standard solution preparation

[0067] Acetonitrile, ethyl acetate, and acetone are made into an extract with a volume ratio of 1:1.2:2;

[0068] Toluene, o-xylene, p-xylene, m-xylene, DMF and DMSO are prepared with extracts at a concentration of 2.0×10 4 6 standard stock solutions of mg / L. Then use the extract to make the concentration of benzene series, DMF, and DMSO respectively 2.0×10 2 mg / L, 1.0×10 3 mg / L, 2.0×10 3 mg / L mixed standard working solution.

[0069] S23, sample pretreatment

[0070] S23.1. Soil sample pretreatment

[0071] Weigh the homogenized soil and add water and extract mixed solution successively according to the solid-to-liquid ratio of 1g: 0.25mL: 2.25mL and mix well, add anhydrous Na 2 SO 4 and mix well, after standing still, centrifuge to get the supernatant and filter to obtain the soil extract.

[0072] Take 2mL soil extract and add anhydrous MgSO 4 , 0.2μm membran...

Embodiment 3

[0081] S31. Instruments and reagents

[0082] Same as S11.

[0083] S32. Standard solution preparation

[0084] Acetonitrile, ethyl acetate, and acetone are formulated into an extract with a volume ratio of 1:1.2:0.5;

[0085] Toluene, o-xylene, p-xylene, m-xylene, DMF and DMSO are prepared with extracts at a concentration of 2.0×10 4 6 standard stock solutions of mg / L. Then use the extract to make the concentration of benzene series, DMF, and DMSO respectively 2.0×10 2 mg / L, 1.0×10 3 mg / L, 2.0×10 3 mg / L mixed standard working solution.

[0086] S33, sample pretreatment

[0087] S33.1. Pretreatment of soil samples

[0088] Weigh the homogenized soil and add water and extract mixed solution successively according to the solid-to-liquid ratio of 1g: 0.25mL: 0.75mL and mix well, add anhydrous Na 2 SO 4 and mix well, after standing still, centrifuge to get the supernatant and filter to obtain the soil extract.

[0089] Take 2mL soil extract and add anhydrous MgSO 4 , 0.2...

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Abstract

The invention relates to the fields of pesticide adjuvant residue detection, drug detection, environmental safety and the like, in particular to a method for detecting residual organic solvents in soil and water by adopting a gas chromatography-mass spectrometry method. The method comprises the following steps that 1, the soil and water to be detected are respectively subjected to solvent extraction and anhydrous Na2SO4 pretreatment and then are centrifuged, supernatant is obtained and filtered to obtain an extraction solution; 2, the gas chromatography-mass spectrometry is adopted to detect the extraction solution in the step 1, wherein a used gas chromatography column is a DB-WAX capillary chromatographic column, and MgSO4 is added in the extraction solution before the chromatographic column is used. Organic solvents include toluene, xylene, DMF and DMSO. The xylene includes dimethylbenzene, paraxylene and dimethylbenzene. The method is fast, convenient and accurate and sensitively detects organic solvent residue quantity in environmental samples such as soil and water.

Description

technical field [0001] The invention relates to the fields of pesticide adjuvant residue detection, drug detection, environmental safety and the like, in particular to a method for detecting organic solvent residues in soil and water by gas chromatography-mass spectrometry. Background technique [0002] Organic solvents are essential chemicals in the production and application of pesticides, chemicals, and pharmaceuticals. Toluene, xylene, DMF, and DMSO are typical organic solvents that are used in large amounts. my country is the country that consumes the largest amount of pesticides in the world. Toluene, xylene, dimethylformamide (DMF), and dimethylsulfame (DMSO) are commonly used as solvents, co-solvents, and stabilizers in pesticide preparations. According to reports, about 400,000 tons of organic solvents such as toluene and xylene are used in the preparation of emulsifiable concentrate in my country every year. DMF is an excellent industrial organic solvent, which can...

Claims

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Application Information

Patent Timeline
22 Mar 2017
Publication
CN106526018A
IPC
G01N30/02; G01N30/72
CPC
G01N30/02; G01N30/7206
Inventors
王珊珊; 王静