人体尿液中芬太尼及其代谢物的固相萃取-气相色谱-串联质谱(SPE-GC-MS)定性定量分析方法研究

STUDY ON THE QUALITATIVE AND QUANTITATIVE ANALYSIS METHOD OF FENTANYL AND NORFENTANYL IN HUMAN URINE BY SPE-GC-MS

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.