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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

Active Publication Date: 2017-03-22
INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

(2) Although a lot of research has been done at home and abroad on the detection technology of toluene, xylene and other benzene series in water bodies, medicines, cosmetics, food packaging, textiles, and architectural coatings, most of them use headspace sampling, which has great influence on the equipment. Certain requirements, higher promotion costs
Moreover, the current research methods mostly use the total amount of xylene to calculate. Although the chemical structures of o-, p-, and m-xylene are very similar, the spatial positions of the two methyl groups have a significant impact on the electron cloud of the benzene ring, resulting in Their chemical properties are very different. For example, p-xylene will be metabolized into p-toluic acid in the human body, and then react with glycine to form methylhippuric acid, which is excreted in urine. Its toxicity is much higher than that of the other two xylenes. Exposure to or short-term access to high concentrations of this substance will cause serious harm to the human body, and it is of great significance to realize the distinction between ortho, meta and p-xylene
(3) Due to the large difference in boiling point and polarity of toluene, xylene, DMF, and DMSO, there are few reports on the analytical methods for accurately and sensitively analyzing organic solvents such as toluene, xylene, DMF, and DMSO at the same time. The method of the sample has not been reported

Method used

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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

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/7206
Inventor 王珊珊王静佘永新金芬邵华金茂俊郑鹭飞
Owner INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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