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一种监测灭梭威(4-(甲硫基)-3,5-二甲苯基-N-甲基氨基甲酸酯)及其亚砜和砜代谢物以及它们在矮丛蓝莓中残留情况的快速气相色谱法。

A rapid GC method of monitoring Mesurol (4-(methylthio)-3,5-xylyl-N-methyl carbamate) and its sulfoxide and sulfone metabolites and their persistence in lowbush blueberries.

作者信息

Greenhalgh R, Wood G W, Pearce P A

出版信息

J Environ Sci Health B. 1977;12(4):229-44. doi: 10.1080/03601237709372067.

Abstract

A facile analytical procedure was developed for determining Mesurol (4-(methylthio)-3,5-xylyl-N-methyl carbamate) and its oxidation products in blueberries. It involved blending with acetone, partition with chloroform and derivatization with trifluoroacetic anhydride and quantitation by gas chromatography/flame photometric detector (GC/FPD). The method showed good recoveries for Mesurol and its sulfoxide at the 0.1 ppm level and Mesurol sulfone at the 0.3 ppm level with a 25 g sample. It was applied to monitor levels of the insecticide and its oxidation products on field-treated blueberries. The sensitivity of the method may be increased 5-fold by the inclusion of a clean-up step. The optimal conditions for the detection of Mesurol TFA by the modified Bendix sulphur/phosphorus emission detector operating in the sulphur mode required an oxygen/hydrogen ratio of 0.38, for a column flow of 60 ml/min. The minimum detectable amounts of the TFA derivatives of Mesurol, its sulfoxide and sulfone were calculated as 1.3, 2.3 and 5.8 X 10(-11) g/sec, respectively.

摘要

开发了一种简便的分析方法,用于测定蓝莓中的灭梭威(4-(甲硫基)-3,5-二甲苯基-N-甲基氨基甲酸酯)及其氧化产物。该方法包括与丙酮混合、用氯仿萃取、用三氟乙酸酐衍生化,并通过气相色谱/火焰光度检测器(GC/FPD)进行定量分析。对于25克样品,该方法在0.1 ppm水平下对灭梭威及其亚砜以及在0.3 ppm水平下对灭梭威砜均显示出良好的回收率。该方法用于监测田间处理过的蓝莓上杀虫剂及其氧化产物的含量。通过增加一个净化步骤,该方法的灵敏度可提高5倍。在硫模式下运行的改进型本迪克斯硫/磷发射检测器检测灭梭威三氟乙酸酯的最佳条件是,氧气/氢气比为0.38,柱流速为60毫升/分钟。灭梭威及其亚砜和砜的三氟乙酸酯衍生物的最低检测量分别计算为1.3、2.3和5.8×10⁻¹¹克/秒。

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