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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 for the simultaneous determination of ten organophosphate toxicants in whole blood samples was established by pretreatment combined with on-line gel chromatography-gas chromatography-mass spectrometry (GPC-GC / MS) based on the principle of matrix dispersion solid-phase extraction. After pretreatment, the whole blood sample can be directly injected without concentration and volumetric preparation, effectively shortening the time-consuming pretreatment, and GPC using a large volume injection mode, which reduces the detection limit and improves the sensitivity compared with the traditional method . Under the optimized experimental conditions, all analytes showed good linearity (R = 0.9990 ~ 0.9999) within the range of 0.5-5 mg / L with a detection limit of 2.2-15.4 mg / L (signal to noise ratio S / N = 3) , The blank spike continuous injection 6 times, the resulting chromatographic retention time and peak area relative standard deviation were less than 3%, the spike recovery was 80.4% ~ 111.7%. The experimental results show that the method is fast and convenient and can meet the detection requirements of organophosphate poisons in actual criminal investigation.