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Method for detecting O, O-dimethyl thiophosphoramide in soil

A technology of dimethyl thiophosphoramide and detection method, which is applied in the field of environmental analysis, can solve the problems of few detection reports, long half-life of pesticides, etc., and achieves the effects of simple operation, reduced matrix interference, and fast and simple processing method.

Pending Publication Date: 2020-09-11
中科检测技术服务(广州)股份有限公司
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Problems solved by technology

[0002] O,O-dimethylphosphorothioate is an intermediate in the production of organophosphorus pesticides. Although some highly toxic organophosphates have been banned in recent years, due to the large production tonnage and many manufacturers in my country, and the long half-life of such pesticides, It is persistent, so it can still be detected in soil, water, and agricultural products. At present, there are reports on the detection methods of organic phosphorus such as temperament and liquid quality at home and abroad. However, for the intermediate O, O-dimethylphosphorothioate There are few reports on the detection of amides

Method used

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  • Method for detecting O, O-dimethyl thiophosphoramide in soil
  • Method for detecting O, O-dimethyl thiophosphoramide in soil
  • Method for detecting O, O-dimethyl thiophosphoramide in soil

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Embodiment 1

[0035] The target compound O, O-dimethyl phosphoramidothioate (O, O-Dimethyl phosphoramidothioate, 87%) was purchased from Chemservice Company; the methanol used in the laboratory was chromatographically pure, anhydrous sodium sulfate was domestic analytical grade, diatomaceous earth for industrial grade. The water is the first-class water specified in GB / T 6682.

[0036] The analytical balance is a ten-thousandth balance (Sartorius, BSA224S-CW); the extraction instrument is a vortex mixer (Haimen Qilinbeier Instrument Manufacturing Co., Ltd., XW-804); the centrifuge is a desktop high-speed refrigerated centrifuge (Hunan Xiang Instrument Laboratory Instrument Development Co., Ltd., TGL-16M); the detection instrument is a liquid chromatography mass spectrometer (Shimadzu, Japan, LCMS8045).

[0037] (1) Sample pretreatment

[0038] Collect soil samples from a factory plot in Guangzhou to remove larger impurities such as stones, roots and leaves, take air-dried soil samples, an...

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Abstract

The invention belongs to the technical field of environmental analysis, and particularly discloses a method for detecting O, O-dimethyl phosphorothioate in soil. The method comprises the following steps: (1) collecting a soil sample, and removing impurities; (2) extracting the pretreated sample by using methanol, specifically, weighing the granular soil sample, adding the methanol, uniformly mixing, then carrying out centrifugal treatment, taking a supernatant, passing through an organic phase nylon filter membrane, and waiting for LC-MS / MS detection; (3) preparing to obtain O, O-dimethyl phosphorothioamide standard working solutions with gradient concentrations; and (4) analyzing and detecting by using a high performance liquid chromatography-triple quadrupole tandem mass spectrometer. According to the method, the recovery rate of the O, O-dimethyl thiophosphoramide ranges from 90% to 100%. And the detection limit of the O, O-dimethyl thiophosphoramide is less than or equal to 0.89 ng / g. The method is suitable for detecting the residual amount of the O, O-dimethyl thiophosphoramide in the soil.

Description

technical field [0001] The invention belongs to the technical field of environmental analysis, in particular to a method for detecting O,O-dimethylphosphorothioate in soil. Background technique [0002] O,O-dimethylthiophosphoramide is an intermediate in the production of organophosphorus pesticides. Although some highly toxic organophosphates have been banned in recent years, due to the large production tonnage and many manufacturers in my country, and the long half-life of such pesticides, It is persistent, so it can still be detected in soil, water, and agricultural products. At present, there are reports on the detection methods of organic phosphorus such as temperament and liquid quality at home and abroad. However, for the intermediate O,O-dimethylphosphorothioate There are few reports on the detection of amides. As an intermediate of organophosphorus pesticides, O,O-dimethylphosphorothioate may enter soil, water and other environments with the use of organophosphorus p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 刘瑞陈晓丹赖华杰张傲赵嘉辉黄晓玲黄靖桐
Owner 中科检测技术服务(广州)股份有限公司
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