摘要
目的獉獉:建立人体尿液中芬太尼(fentanyl)及其代谢物去苯乙基芬太尼(norfentanyl)的SPE-GC-MS定性定量检测分析方法。方法獉獉:人体尿液样本采用固相萃取法进行提取,用HFBA试剂衍生后,用气相色谱-质谱仪在电子电离模式下检测样本中的芬太尼及其代谢物,通过同位素内标方法进行定量分析,从抗干扰性、精密度、回收率等方面进行验证。结果獉獉:方法中芬太尼的最低检出量为5.0 ng.mL-1;定量线性范围为100.0-1600.0 ng.mL-1,最低定量限为20.0 ng.mL-1;在300.0 ng.mL-1和1000.0 ng.mL-1的浓度下的日内精密度分别为3.15%和2.65%(n=6),日间精密度为3.01%和2.83%(n=6);在200.0 ng.mL-1和800.0 ng.mL-1浓度下,前处理回收率分别为97.19%和102.22%(n=3);去苯乙基芬太尼的最低检出量为1.0 ng.mL-1;定量线性范围为100.0-1600.0 ng.mL-1,最低定量限为20.0 ng.mL-1;在300.0 ng.mL-1和1000.0 ng.mL-1的浓度下的日内精密度分别为1.25%和1.88%(n=6),日间精密度为1.56%和1.43%(n=6);在200.0 ng.mL-1和800.0 ng.mL-1浓度下,前处理回收率分别为96.92%和100.12%(n=3)。结论獉獉:本方法是一种准确、灵敏、特异性好的检测方法,可用于药物滥用人员尿液中芬太尼及其代谢物的定性定量分析。
Objective:To set up a method for the qualitative and quantitative analysis of fentanyl and its metabolite norfentanyl in human urine by solid -phase extraction and gas chromatography -mass spectrometry (SPE -GC -MS). Met.h.ods...:grine samples and the standard curve solutions were prepared by the SPE extraction and HFBA derivatization. The final extract was determined by GC -MS with electron impact ion source, and internal standard -standard curve quantitative method was used for analysis. The method was verified with anti -interference, precision, and the percentage recovery. Results : Fentanyl : the limit of detection was 5.0 ng ~ mL- 1 ; the quantitative linear range was 100.0 - 1600.0 ng ~ mL- 1 ; the limit of quantitation was 20.0 ng· mL- 1 ;the intra - day precision of the assays at 300.0 ng ·mL-l and 1000.0 ng · mL-1 was 3.15% and 2.65% (n =6) , and inter -day precision was 3.01% and 2.83 % ( n = 6), respectively ; the percentage recovery at 200.0 ng · mL- 1 and 800.0 ng· mL-1 was 97.19% and 102.22% ( n = 3) respectively. Norfentanyl :the limit of detection was 1.0 ng ·mL-1 ;the quantitative linear range was 100.0 - 1600.0 ng · mL-1 ;the limit of quantitation was 20.0 ng· mL-1 ;the intra - day precision of the assays at 300.0 ng · mL-j and 1000.0 ng · mL-1 was 1.25% and 1.88% (n =6), and inter - day precision was 1.56% and 1.43% (rt =6), respectively;the percentage recovery at 200.0 ng·mL-1 and 800.0 ng· mL-1 was 96.92% and 100, 12% ( n = 3 ) respectively. Conclusion : The SPE - GC - MS procedure is precise, sensitive and specific. It is an effective method for the qualitative and quantitative analysis of fentanyl and norfentanyl in urine of drug abusers.
出处
《中国药物依赖性杂志》
CAS
CSCD
2013年第4期271-275,共5页
Chinese Journal of Drug Dependence