Szostek B, Aldstadt J H
Environmental Research Division, Argonne National Laboratory, IL 60439-4843, USA.
J Chromatogr A. 1998 May 22;807(2):253-63. doi: 10.1016/s0021-9673(98)00080-6.
The development of a method for the analysis of organoarsenic compounds that combines dithiol derivatization with solid-phase microextraction (SPME) sample preparation and gas chromatography-mass spectrometry (GC-MS) is described. Optimization focused on a SPME-GC-MS procedure for determination of 2-chlorovinylarsonous acid (CVAA), the primary decomposition product of the chemical warfare agent known as Lewisite. Two other organoarsenic compounds of environmental interest, dimethylarsinic acid and phenylarsonic acid, were also studied. A series of dithiol compounds was examined for derivatization of the arsenicals, and the best results were obtained either with 1,3-propanedithiol or 1,2-ethanedithiol. The derivatization procedure, fiber type, and extraction time were optimized. For CVAA, calibration curves were linear over three orders of magnitude and limits-of-detection were < 6.10(-9) M in solution, the latter a more than 400 x improvement compared to conventional solvent extraction GC-MS methods. A precision of < 10% R.S.D. was typical for the SPME-GC-MS procedure. The method was applied to a series of water samples and soil/sediment extracts, as well as to aged soil samples that had been contaminated with Lewisite.
本文描述了一种结合二硫醇衍生化、固相微萃取（SPME）样品制备和气相色谱-质谱联用（GC-MS）的有机砷化合物分析方法的开发。优化工作聚焦于一种用于测定2-氯乙烯基亚胂酸（CVAA）的SPME-GC-MS程序，CVAA是化学战剂路易氏剂的主要分解产物。还研究了另外两种具有环境意义的有机砷化合物，二甲基胂酸和苯胂酸。考察了一系列二硫醇化合物用于砷化合物的衍生化，使用1,3-丙二硫醇或1,2-乙二硫醇可获得最佳结果。对衍生化程序、纤维类型和萃取时间进行了优化。对于CVAA，校准曲线在三个数量级上呈线性，溶液中的检测限<6.10(-9) M，与传统溶剂萃取GC-MS方法相比，后者有超过400倍的改进。SPME-GC-MS程序的典型相对标准偏差（R.S.D.）<10%。该方法应用于一系列水样、土壤/沉积物提取物以及曾被路易氏剂污染的老化土壤样品。
