GC/MS、GC/NPD法检测毛发中的氯胺酮

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。

Determination of ketamine in hair by gas chromatography/mass spectrum and gas chromatography/nitrogen phosphor detector

Objective Rapid and sensitive methods were developed for identification and quantitation of hair ketamine by GC/MS and GC/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/β-glucuronidase.The effect of different digestion methods and extraction solvents 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 0.1ng/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.