急性磷化物中毒检材的顶空气相色谱快速确证方法

Rapid identification of acute phosphide poisoning by headspace gas chromatography

目的建立一种简便、快速、准确的顶空进样气相色谱法,检测血样及食品等中毒检材中的磷化物。方法含有磷化物及其代谢物亚磷酸的中毒检材在硫酸及锌粉作用下生成磷化氢,样品经过简单处理即可采用顶空进样结合气相色谱法分离及磷型火焰光度检测器进行检测,保留时间定性,峰面积、外标法定量。结果通过优化前处理过程中硫酸的加入量及加入浓度、锌粉的加入量、顶空平衡温度和平衡时间等条件,磷化氢在0.10μg~20.0μg内线性关系良好,相关系数为0.9993,对牛全血样品的加标回收率为89.0%~113.1%,相对标准偏差(RSD)为3.2%~8.7%。按取样量为1.0 g计,方法检出限为0.03μg/g,定量限为0.1μg/g。结论本方法具有前处理操作步骤简单,检出限低,可快速定性及高灵敏定量检测的优点,可用于中毒者血样和食物中毒检材中磷化物的检测。

Objective To establish a simple,rapid and accurate analytical method for identification of phosphide in acute poisoning exhibits including blood and food samples by headspace gas chromatography.Methods Phosphide and its metabolite phosphite in poisoning exhibits generated phosphine in the presence of sulfuric acid and zinc dust.After simple pretreatment for the reaction system,phosphine was separated and detected by headspace gas chromatography with phosphorus flame photometric detector.The retention time was used for qualitative analysis.Meanwhile,peak areas were used for quantitative analysis using external standard method.Results By optimizing the amounts and concentration of sulfuric acid,the amounts of zinc used,as well as the equilibrium temperature and time,phosphine was linear in the range of 0.10μg-20.0μg with the correlation coefficient of 0.9993.The recoveries for spiked bovine whole blood samples were between 89.0%and 113.1%,with the corresponding relative standard deviations(RSDs)in the range of 3.2%-8.7%.When 1.0 g of sample was used,the limit of detection(LOD)and the limit of quantification(LOQ)was 0.03μg/g and 0.1μg/g,respectively.Conclusion The established method has the merits of simple sample pretreatment,low detection limit,rapid identification and high sensitivity.It is applicable for phosphine identification in exhibits such as the poisoner’s blood and food poisoning samples.