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气相色谱法测定个人防护装备中的倍硫磷及其氧化产物

Determination of fenthion and oxidation products in personal protection equipment by gas chromatography.

作者信息

Tsakirakis Angelos, Machera Kyriaki

机构信息

Laboratory of Pesticides Toxicology, Benaki Phytopathological Institute, 8 St. Delta Street, Kifissia 14561, Athens, Greece.

出版信息

J Chromatogr A. 2007 Nov 9;1171(1-2):98-103. doi: 10.1016/j.chroma.2007.09.019. Epub 2007 Sep 14.

Abstract

A method for the co-extraction and simultaneous chromatographic determination of fenthion and its five oxidation products (or metabolites) fenoxon, fenoxon-sulfoxide, fenoxon-sulfone, fenthion-sulfoxide, and fenthion-sulfone in personal protection equipment (PPE) of pesticide applicators was developed and validated. Capillary gas chromatography-nitrogen-phosphorus detection was used for the analytical determination of all the aforementioned compounds over the concentration range of 0.1-0.5 microg/mL. All necessary validation criteria of the method were met. The method was found to be highly selective, accurate, and precise, gave satisfactory recovery (>70%) and RSD values (<20%) for fenthion and its metabolites in all tested specimens of personal protection equipment and in air samplers. The limit of quantification (LOQ) and linearity were determined for the most relevant PPE (i.e. inner coverall) for the parent compound and for the metabolites. The LOQ values ranged from 0.05 to 0.1 ppb while the linearity in the tested range of 0.1-0.5 ppm had r(2)>0.994 for all analytes.

摘要

开发并验证了一种用于同时萃取和色谱测定农药施用人员个人防护装备(PPE)中倍硫磷及其五种氧化产物(或代谢物)即氧乐果、氧乐果亚砜、氧乐果砜、倍硫磷亚砜和倍硫磷砜的方法。采用毛细管气相色谱 - 氮磷检测法对上述所有化合物在0.1 - 0.5微克/毫升的浓度范围内进行分析测定。该方法满足了所有必要的验证标准。结果发现该方法具有高度选择性、准确性和精密度,在所有测试的个人防护装备样本和空气采样器中,倍硫磷及其代谢物的回收率令人满意(>70%),相对标准偏差值(<20%)。针对母体化合物及其代谢物,测定了最相关的个人防护装备(即内工作服)的定量限(LOQ)和线性度。定量限的值在从0.05到0.1 ppb之间,而在0.1 - 0.5 ppm的测试范围内,所有分析物的线性度r(2)>0.994。

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