固相萃取-气相色谱-质谱联用法测定人血清中甲胺磷和乙酰甲胺磷

Determination Of Methamidophos And Acetphate In Human Serum by Solid Phase Extraction Gas Chromatography-Mass Spectrometry

目的建立一种人血清中乙酰甲胺磷及其代谢物甲胺磷的测定方法,即固相萃取-气相色谱-质谱联用法。方法取0.3ml待测血清,用去离子水稀释至3ml,经固相萃取小柱(Carb柱,400mg)提取,目标化合物经丙酮洗脱,氮气吹干后,加入10μl的内标物(苯酚),再用丙酮定容至1ml,取1μl进样。结果甲胺磷和乙酰甲胺磷的线性范围分别为20～100mg/L和10～80mg/L;方法的加标回收率范围为:92.1%～114%;RSD为:3.5%-10.4%。当取样量为0.3ml时,甲胺磷和乙酰甲胺磷的最低检出限分别为10 mg/L和5 mg/L。结论该方法分析快速,定性、定量准确,完全能满足突发性中毒事件的确证分析。

Objective To explore a determination method of acetphate and methamidophos in human serum, that is solid phase extraction gas chromatography - mass spectrometry （ GC - MS）. Methods 0.3ml Sera to be assayed were taken and diluted to 3ml with the deionized waterp and were extracted and purified by Carb 400 column. After the eluation of acetone and the blow dry of nitrogen, the titled compounds were settled to the volume of 1 ml through adding into 10 μl Phenol which was thought to be internal standard, then 1μ1 sample was injected into GC - MS for analysis. Results The linear range for the determination of methamidophos and aeetphate were 20 - 100 mg/L and 10 - 80 mg/L respectively. The recovery of standard addition of the samples was 92.1% - 114%. The relative standard deviation （ RSD ） was 3.5 % - 10.4%. The lowest detection limits of methamidophos and acetphate were 10 mg/L and 5 mg/L respectively when the 3ml sample was analyzed. Conclusion This method was rapid, accurate quantitatively and qualitatively, could satisfactorily meet the requirements of confirmatory analysis of emergency poisoning accidents.