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超临界流体萃取-氮磷检测气相色谱法测定小麦粉中的有机磷农药

Determination of organophosphorus pesticides in wheat flour by supercritical fluid extraction and gas chromatography with nitrogen-phosphorus detection.

作者信息

Kim D H, Heo G S, Lee D W

机构信息

Organic Analytical Laboratory, Korea Research Institute of Standards and Science, Daejon, South Korea.

出版信息

J Chromatogr A. 1998 Oct 16;824(1):63-70. doi: 10.1016/s0021-9673(98)00629-3.

Abstract

Application of supercritical fluid extraction (SFE) for selective isolation of organophosphorus pesticides from a real-world matrix (wheat flour) has been described. The method uses extraction with supercritical carbon dioxide at 206.8 bar and 60 degrees C, followed by quantitation by gas chromatography with nitrogen-phosphorous detection without clean-up of the extracts. Comparison of SFE with a method currently employed for sample preparation (i.e., organic solvent extraction followed by liquid-liquid extraction and gel permeation chromatography clean-up) shows that the SFE technique simplifies the sample preparation step and speeds up the determination of organophosphorus pesticides in flour. Extraction times were 60 min for a 7 g sample size. This technique was able to determine organophosphorus pesticides (ethoprophos, diazinon, chlorpyrifos methyl, fenitrothion, parathion, phenthoate, EPN) in samples at the 10 ng/g level.

摘要

已描述了超临界流体萃取(SFE)用于从实际基质(小麦粉)中选择性分离有机磷农药的应用。该方法采用在206.8巴和60摄氏度下用超临界二氧化碳进行萃取,随后通过带有氮磷检测的气相色谱法定量,提取物无需净化。将SFE与目前用于样品制备的方法(即有机溶剂萃取,随后进行液液萃取和凝胶渗透色谱净化)进行比较表明,SFE技术简化了样品制备步骤,并加快了面粉中有机磷农药含量的测定。对于7克的样品量,萃取时间为60分钟。该技术能够测定样品中含量为10纳克/克水平的有机磷农药(丙线磷、二嗪农、甲基毒死蜱、杀螟硫磷、对硫磷、稻丰散、硫环磷)。

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