气/质联用和气相色谱-NPD法分析唾液中哌替啶

Analysis of pethidine in saliva by GC / MS and GC-NPD

目的 建立唾液中哌替啶的提取方法以及气相色谱-质谱和气相色谱-NPD分析方法.方法 实验家兔静脉注射哌替啶,于注射后15 ～ 600min之间的10个时间点收集唾液样品;样本加入内标物利多卡因,采用有机溶剂萃取后,进行气相色谱-质谱联用（GC/MS）定性分析、气相色谱-NPD定量分析唾液中哌替啶浓度.并对不同pH条件和不同有机溶剂萃取剂以及方法学进行考察.结果 在pH12条件下使用二氯甲烷萃取唾液中哌替啶效果较好.唾液中哌替啶气相色谱-NPD分析方法线性检测范围为2.0～100.0μg/mL,相关系数0.995 0,最低检出限为2.0μg/mL,回收率范围98.80％ ～ 114.72％,日内和日间精密度均小于2.88％.结论 建立的唾液中哌替啶气/质联用和气相色谱-NPD分析方法,可用于哌替啶中毒与滥用的快速检验鉴定.

Objective A method for analyzing of pethidine in saliva samples by GC/MS and GC-NPD was developed. Methods The rabbits in experimental groups were given intravenous injection of pethidine and the sample taken from the saliva of the rabbits were collected at 10 time points within 15 - 600 minutes after injection. The saliva samples were alkalified and extracted by dichloromethane after adding lidocaine （internal standard, IS）. The extracts were qualitatively analyzed by GC/MS and quantitatively analyzed by GC-NPD. The experiment has investigated pH conditions and extraction solvent. Results The best extraction condition of pethidine in saliva was selected at pH 12, and extracted by dichloromethane. The linear range for pethidine in saliva was 2.0 ～ 100. 0μg/mL. The limit of detection was 2.0μg/mL. The analytical recovery was 98.80% ～ 114.72%. The inter-and intra-day relative standard deviations of precisions were less than 1.16 %. Conclusion The method of analyzing of pethidine in saliva samples can be used for identification of poisoning of pethidine and pethidine abuse.