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作 者:朱军[1] 邸玉敏[2] 常靖[1] 崔巍[1] 于忠山[1] 刘耀[1]
机构地区:[1]公安部物证鉴定中心,北京100038 [2]天津市公安局禁毒总队,天津300240
出 处:《中国法医学杂志》2013年第3期184-187,共4页Chinese Journal of Forensic Medicine
基 金:十一五国家科技支撑计划项目(2006BAK09B06)
摘 要:目的采用液-液萃取、衍生化和GC/MS、GC/NPD方法,进行毛发中氯胺酮定性定量分析。方法选择4-苯基丁胺为内标,毛发样本用NaOH、HCl及芳基硫酸酯酶/β-葡萄糖醛酸酶等3种方式进行水解,再进行衍生化后,采用GC/MS和GC/NPD方法定性定量分析。对不同水解和衍生化条件以及提取溶剂进行比较优化,并考察方法精密度、稳定性和检出限。结果方法的提取回收率大于95%,精密度和样品稳定性良好,日内和日间标准偏差小于6%;采用GC/NPD和GC/MS直接分析毛发中的氯胺酮,检出限为0.2ng/mg和2.0ng/mg,线性范围为10.0~250.0ng/mg,相关系数均大于0.99;采用酰化衍生化后分析,GC/NPD和GC/MS检出限分别提高至0.1ng/mg和0.2ng/mg。结论该方法回收率高、检测限低,可以用于毛发中氯胺酮的定性定量分析检验。[ Abstract] Objective Rapid and sensitive methods were developed for identification and quantitation of hair ketamine by GC/MS and CC/NPD with liquid-liquid extraction and derivatization. Methods Using 4-PBA as the internal standard, hair was digested by sodium hydroxide, hydrochloric acid, or arylsulfatase/- glucuronidase. The effect of different digestion methods and extraction solverits for extraction recovery was studied and comparied. The detection methods of hair ketamine were developed by GC/MS and GC/NPD with liquid-liquid extraction. Results Experimental results indicated that the recovery of hair ketamine was larger than 95%, relative standard deviations of intra-day and inter-day were less than 6%. Limits of identification for hair ketamine were 0. 2ng/mg and 2. 0ng/mg by GC/NPD and GC/MS respectively. The standard curves were linear in the range of 10. 0ng/mg to 250. 0ng/mg with correlation coefficients larger than 0. 99. After acetylation treatment, limits of hair ketamine were 0. 1 ng/mg and 0.2ng/mg by GC/NPD and GC/MS respectively.Conclusion The methods are particularly useful for qualitative and quantitative analysis of hair ketamine.
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