人毛发中36种芬太尼类物质的HPLC-MS/MS检测方法

建立了同时对人毛发中36种芬太尼类物质快速定性定量检测方法,并成功应用于实际案件的检测.利用高效液相色谱-串联质谱(HPLC-MS/MS)技术,采用MRM(多反应监测)模式,用Waters ACQUITY BEH C18(100mm×2.1 mm,1.7 μm)色谱柱,柱温50℃,流动相为甲醇-0.1％甲酸的水溶液(V...

Determination of 36 Fentanyl Analogs in Human Hair by HPLC-MS/MS

Objective A rapid qualitative and quantitative method for the detection of 36 fentanyl analogs in human hair simultaneously was established,and this method was applied in actual cases.Methods The hair sample was determined by HPLC-MS/MS using MRM(multiple reaction monitor)mode,and separated on chromatographic column Waters ACQUITY BEH C18(100 mm×2.1 mm,1.7μm)with mobile phase consisting of methanol-aqueous solution of 0.1%formic acid(V/V),gradient elution.The hair samples were washed with 0.1%SDS,water and acetone successively.Then the hair samples were ground into a powder,weighted 20 mg,soaked with 1mL methanol for 18h,added 1mL deionized water,mixed and filtrated the solution with filter membrane,analyzed the solution using HPLC-MS/MS.Results 36 fentanyl analogs can be separated effectively,including that baseline separation of 3 pairs of isomers were achieved.The detection limits of 36 fentanyl analogs were all 0.01 ng·mg^-1.The retention time RSDs were less than 0.33%.The quantitative detection was conducted on Fentanyl and Alfentanil,the linear ranges are all 0.01~2 ng.mg^-1,and the correlation coefficient were 0.997 and 1 respectively.When the spiked levels were 0.05、0.2、1 ng·mg^-1,the average recoveries were between 89.34%~104.80%,the matrix effect was in the range of 96.95%~112.59%,the rang of accuracy was 91.92%~102.34%,the ranges of intraday and interday relative standard deviations(RSDs)were 0.49%~6.84%and 1.21%~7.00%respectively.Conclusion The method is simple,efficient,accurate and sensitive and it can be used as a monitoring method for the abuse of fentanyl substance.