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顶空固相微萃取气相色谱/质谱法测定大鼠血浆和脑组织中的二异丙基氟磷酸酯

Determination of diisopropylfluorophosphate in rat plasma and brain tissue by headspace solid-phase microextraction gas chromatography/mass spectrometry.

作者信息

Xu Meng, Terry Alvin V, Bartlett Michael G

机构信息

Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USA.

出版信息

Rapid Commun Mass Spectrom. 2008 Oct;22(19):3069-75. doi: 10.1002/rcm.3706.

Abstract

A simple, sensitive and rapid method for the determination of diisopropylfluorophosphate (DFP) in rat plasma and brain tissue using headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS) is presented. A 65 microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was selected for sampling. The main parameters affecting the SPME process such as extraction and desorption temperature, extraction and desorption time, salt addition, and fiber preheating time were optimized in each matrix to enhance the extraction efficiency of the method. The lower limits of quantitation for DFP in plasma and brain tissue were 1 ng/mL and 3 ng/g, respectively. The method showed good linearity over the range from 1-100 ng/mL in plasma and 3-300 ng/g in brain tissue with correlation coefficient (R(2)) values higher than 0.995. The precision and accuracy for intra-day and inter-day were less than 10%. The relative recoveries in plasma and brain for DFP were greater than 50%. Stability tests including autosampler and freeze and thaw were also investigated. This validated method was successfully applied to study the neurobehavioral effects of low-level organophosphate exposures.

摘要

本文介绍了一种使用顶空固相微萃取(HS-SPME)和气相色谱/质谱联用(GC/MS)测定大鼠血浆和脑组织中磷酸二异丙酯(DFP)的简单、灵敏且快速的方法。选用了65微米的聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)纤维进行采样。针对每个基质,对影响固相微萃取过程的主要参数,如萃取和解吸温度、萃取和解吸时间、加盐量以及纤维预热时间进行了优化,以提高该方法的萃取效率。血浆和脑组织中DFP的定量下限分别为1 ng/mL和3 ng/g。该方法在血浆中1 - 100 ng/mL以及脑组织中3 - 300 ng/g的范围内呈现出良好的线性,相关系数(R²)值高于0.995。日内和日间的精密度和准确度均小于10%。DFP在血浆和脑组织中的相对回收率大于50%。还研究了包括自动进样器以及冻融在内的稳定性测试。该经过验证的方法成功应用于研究低水平有机磷暴露的神经行为效应。

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