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目的建立人血液、肝脏中杀扑磷的气相色谱快速分析方法。方法收集血、肝样本,采用有机溶剂萃取后,进行气相色谱(GC)分析,对样本中的杀扑磷进行定性、定量。对提取溶剂、内标物等方法学进行考察和优化,并对1例大剂量口服杀扑磷中毒者死后开棺所取的肝、肾和1例口服杀扑磷急性中毒患者血液浓度进行测定。结果使用正己烷∶乙酸乙酯(7∶3)作为提取溶剂,采用甲基对硫磷作为内标物,进行GC检测分析。血、肝样本中杀扑磷分别在1.0~160.0μg/m L、1.0~160μg/g范围内线性关系良好,r值分别为0.996、0.997;最低检测限分别为0.2μg/m L和0.5μg/g(S/N≥3),精密度日内均小于5%,日间均小于10%;回收率在95.8%~104.4%之间。结论本文分析方法操作便捷、实用、准确度高,适用于杀扑磷的临床中毒抢救和法医毒物鉴定。
Objective To establish a rapid method for the analysis of carbofuran in human blood and liver by gas chromatography. Methods Blood and liver samples were collected and analyzed by gas chromatography (GC) after organic solvent extraction. The methodology of extracting solvent and internal standard was investigated and optimized. The blood concentration of liver, kidney and one case of oral Killer Acute Acute Poisoning in 1 case of high dose oral Killing Phosphorus poisoning Determination. Results n-Hexane: ethyl acetate (7: 3) was used as the extraction solvent and methyl parathion as the internal standard for GC analysis. The linear relationship was obtained between blood and liver samples in the range of 1.0-160.0 μg / mL and 1.0-160 μg / g, respectively, with r values of 0.996 and 0.997, respectively. The limits of detection were 0.2 μg / mL and 0.5 μg respectively / g (S / N≥3). The precision was less than 5% during the day and less than 10% during the day. The recoveries ranged from 95.8% to 104.4%. Conclusion This method is simple, practical and accurate. It is suitable for clinical poisoning and forensic toxicological identification.