论文部分内容阅读
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p H条件和不同有机溶剂萃取剂以及方法学进行考察。结果在p H12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/m L,相关系数0.995 0,最低检出限为2.0μg/m L,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 To establish a method for the extraction of pethidine in saliva and gas chromatography-mass spectrometry and gas chromatography-NPD analysis. Methods The pethidine was intravenously injected into the rabbits and saliva samples were collected at 10 time points between 15 and 600 minutes after injection. The sample was added with lidocaine, which was extracted with organic solvent and then subjected to gas chromatography-mass spectrometry GC / MS) qualitative analysis, gas chromatography-NPD quantitative analysis saliva pethidine concentration. Different p H conditions and different organic solvent extractants and methodology were also investigated. Results The extraction of pethidine in saliva using dichloromethane under p H12 was better. The linear range was 2.0-100.0μg / m L, the correlation coefficient was 0.995 0, the detection limit was 2.0μg / m L, and the recovery range was 98.80% -1 114.72%. The intra-and inter-day Daytime precision less than 2.88%. Conclusion The established method of pethidine gas / mass spectrometry and gas chromatography-NPD analysis in saliva can be used for the rapid test identification of pethidine poisoning and abuse.