Key Laboratory of Evidence Science (China University of Political Science and Law), Ministry of Education, Shijingshan District, Beijing, China.
Forensic Sci Int. 2010 May 20;198(1-3):70-3. doi: 10.1016/j.forsciint.2009.12.053. Epub 2010 Jan 8.
The purpose of our work was to develop a simple and efficient analytical method for simultaneous determination of different species of organic phosphorus pesticides from plasma sample by using automated solid phase extraction (SPE) and gas chromatography/pulsed flame photometric detector (GC/PFPD) as a diagnostic tool. Firstly, the developed extraction method was validated using 5 certified reference materials; then, it was applied to plasma sample. Such factors as the category and volume of wash and elution solvent were examined separately. Among these factors, the category of elution solvent is most important. Hexane-acetone (50:50, v/v) seems to be the best choice for it. The eluent was evaporated on a nitrogen stream at room temperature and redissolved by acetone. 1microL of aliquots was chromatographed on GC/PFPD. Response versus the amount of pesticides injected ranging from 0.05 to 2ng showed a good linearity. The detection limits were 0.01ng for dimethoate, 0.03ng for methyl-parathion and malathion, 0.04ng for terbufos and 0.02ng for parathion. Extraction recoveries range from 84.3% to 109.1%.This extraction method for multispecies analysis incorporates many benefits in terms of speed, low solvent use, accuracy of measurement, sensitivity, relative simplicity, as well as the time saving and convenience of multiple species measurement through sample preparation and analysis as an integrated step.
我们的工作目的是开发一种简单高效的分析方法,通过自动化固相萃取(SPE)和气相色谱/脉冲火焰光度检测器(GC/PFPD)作为诊断工具,同时测定血浆样品中不同种类的有机磷农药。首先,使用 5 种有证参考物质对所开发的提取方法进行验证;然后,将其应用于血浆样品。分别考察了洗涤和洗脱溶剂的种类和体积等因素。在这些因素中,洗脱溶剂的种类最为重要。正己烷-丙酮(50:50,v/v)似乎是最佳选择。在室温下用氮气将洗脱液蒸发,并通过丙酮重新溶解。取 1μL 等分试样在 GC/PFPD 上进行色谱分析。从 0.05 到 2ng 的进样量与农药响应之间呈良好的线性关系。检测限为乐果 0.01ng、甲基对硫磷和马拉硫磷 0.03ng、涕灭威 0.04ng、对硫磷 0.02ng。提取回收率范围为 84.3%至 109.1%。这种用于多物种分析的提取方法在速度、溶剂用量低、测量准确性、灵敏度、相对简单性以及通过样品制备和分析作为一个集成步骤节省时间和方便进行多种物种测量方面具有许多优势。