生物样品中吗啡GC和GC/MS测定方法

Optimizing analysis condition of GC and GC/MS for detecting morphine in biomaterial samples

目的：优化生物样品中吗啡的衍生化条件及气相色谱和气相色谱/质谱定性定量分析条件。方法：吗啡中毒犬血液和肝脏酸水解后,三氯甲烷-异丙醇（9：1）萃取,丙酸酐-吡啶衍生化,气相色谱/质谱联用法定性分析、气相色谱内标法定量检测生物样品中吗啡。结果：吗啡与丙酸酐-吡啶以1：3：2比例、在微波80火力3 min能够完全衍生。心血和肝脏中吗啡气相色谱检测的回归方程、线性检测范围、相关系数、回收率、最低检出浓度分别为Y=0.0796X＋0.0821、0.2~120μg/ml、0.9976、92.6%±0.55%、0.02μg/ml（S/N〉3）和Y=0.0457X＋0.0656、0.2~120μg/ml、0.9955、90.07%±0.67%、0.02μg/ml（S/N〉3）。结论：建立的生物样品中吗啡的气相色谱/质谱检测方法选择性好,灵敏度高,气相色谱定量分析结果准确,可用于吸毒者中毒的临床快速检验和吸毒者中毒死亡案件的法医学鉴定。

Objective：To establish and optimize the derivation and analysis condition of GC and GC/MS for detecting the morphine in biomaterial samples.Methods：The morphine in blood and liver was hydrolyzed and extracted with trichlormethane-isopropanol（9：1）,then was derived with propionic anhydride and analyzed qualitatively and quantitatively by GC/MS and GC,respectively.Results：Morphine could be derived completely under the condition of morphine-propionic anhydride-pydride（1：3：2） and microwave for 3 min.The regression equation,linear range,correlation coefficient,recovery rate,limit of detection of morphine in heart blood and liver were Y=0.0796X＋0.0821,0.2~120 μg/ml,0.9976,92.6±0.55%,0.02 μg/ml and Y=0.0457X＋0.0656,0.2~120 μg/ml,0.9955,90.07±0.67（%）,0.02 μg/ml（S/N3）,respectively.Conclusion：This method for determination of morphine in biomaterial is selective,sensitive and can be applied to not only clinical diagnosis of morphine poisoning,but also forensic identification in morphine poisoning death.