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气相色谱 - 质谱联用法定量分析两种马拉硫磷制剂中的烷基苯惰性成分、农药生产副产物及活性成分

Simultaneous gas chromatographic-mass spectrometric quantitation of the alkylbenzene inert components, pesticide manufacturing by-products and active ingredient in two malathion formulations.

作者信息

Lin Y W, Hee S S

机构信息

Department of Environmental Health Sciences, UCLA School of Public Health 90095-1772, USA.

出版信息

J Chromatogr A. 1998 Jul 24;814(1-2):181-6. doi: 10.1016/s0021-9673(98)00407-5.

DOI:10.1016/s0021-9673(98)00407-5
PMID:9718693
Abstract

A rapid, reliable and effective method for direct determination of the inert components, manufacturing by-products of the pesticide, and active ingredient in two malathion formulations has been established using capillary gas chromatography-mass spectrometry (GC-MS) with the internal standard method. The C2-, C3-, and C4-alkylbenzenes, the major pesticide manufacturing by-products (O,O,S-trimethylthionophosphate, diethyl maleate and O,O,O-trimethylthionophosphate), and malathion were resolved, and quantified in the same chromatogram. Structural identification was based on MS total ion current data, comparison of GC retention times with those of authentic standards, and retention indices. O,O,S-Trimethylthionophosphate was quantified at 3.57 +/- 0.31% (w/w) in one malathion formulation. While the malathion contents were within specifications for both formulations, the total alkylbenzene contents were not.

摘要

采用毛细管气相色谱 - 质谱联用(GC - MS)内标法,建立了一种快速、可靠且有效的方法,用于直接测定两种马拉硫磷制剂中的惰性成分、农药生产副产物及活性成分。主要农药生产副产物(O,O,S - 三甲基硫代磷酸酯、马来酸二乙酯和O,O,O - 三甲基硫代磷酸酯)以及马拉硫磷中的C2 - 、C3 - 和C4 - 烷基苯得以在同一色谱图中分离并定量。结构鉴定基于质谱总离子流数据、将气相色谱保留时间与标准品保留时间进行比较以及保留指数。在一种马拉硫磷制剂中,O,O,S - 三甲基硫代磷酸酯的定量含量为3.57±0.31%(w/w)。虽然两种制剂中马拉硫磷含量均符合规格,但总烷基苯含量不符合。

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