在线凝胶色谱-气相质谱联用法同时快速测定全血样中10种有机磷

Quick simultaneously determination of ten organophosphorus in whole blood using on-line gel permeation chromatography-gas chromatography tandem mass spectrometry

采用基于基质分散固相萃取原理的前处理结合在线凝胶色谱-气相质谱联用技术(GPC-GC/MS),建立了一种同时测定全血样中10种有机磷毒物的定量方法。全血样品经前处理后无需浓缩定容可直接进样,有效缩短前处理耗时,且GPC采用大体积进样模式,联用后相较于传统气质方法降低了检出限并且提高了灵敏度。优化的实验条件下,所有被测物均在0.5~5 mg/L范围内线性良好(R=0.9990~0.9999),检出限为2.2~15.4 mg/L(信噪比S/N=3),将空白加标连续进样6次,得到的色谱保留时间及峰面积相对标准偏差均小于3%,加标回收率为80.4%~111.7%。实验结果表明,该方法便捷快速,能够满足实际刑侦案件中有机磷毒物的检测需求。

A quantitative method employing matrix dispersion extrachon pnnclple as pretreatment was described for the simultaneous determination of ten organophosphorus （methamidophos, dichlorvos, acephate, phorate, dimethoate, disulfoton, parathion-methyl, malathion, parathion and ethion） using on-line gel permeation chromatography-gas chromatography tandem mass spectrometry. The whole blood samples could be injected directly without concentration, which efficiently reduced time consuming during pretreatment. Compared detection and improved the sensitivity for to traditional GC/MS, tandem GPC lowered the limit of its programmed temperature vaporizer. Under optimized experiment condition, a series of standard solutions consisting of target organophosphorus of various concentrations from 0. 5 - 5 mg/L were analyzed, with correlation coefficients 0. 9990 - 0. 9999 and satisfactory repeatabilities （ RSD 〈 3%, n = 6）. The limits of detection were in the range of 2.2- 15.4 mg/L based on S/N of 3, meanwhile recovery rates were between 80. 4% - 111.7%. The results showed that the method was simple and effective, which was suitable for simultaneous determination of organophosphorus in practical cases.