液相色谱-串联质谱法测定固体及液体药物中27种新型毒品芬太尼类物质

Determination of 27 Novel Fentanyl Analogs and Metabolites in Solid and Liquid Drugs by Liquid Chromatography-Tandem Mass Spectrometry

采用QuEChERS法及固相萃取(SPE)法净化样品,结合液相色谱-串联质谱(LC-MS/MS),建立了固体和液体药物中27种新型毒品芬太尼类物质(芬太尼类似物和代谢物)的测定方法。分析物采用电喷雾离子源,正离子多反应监测(MRM)模式检测,外标法定量。结果表明,27种芬太尼类物质在0.5~50.0μg/L质量浓度范围内呈良好线性关系,相关系数(r^2)均大于0.99,方法的定量下限为10.0μg/kg(固体药物)、10.0μg/L(液体药物);3个加标水平的回收率为84.8%~109%;相对标准偏差(RSD)为0.86%~8.5%。该方法快速简便,耗时短,灵敏度高,稳定性好,可用于药物中芬太尼类物质的定性鉴定及定量检测,有助于落实我国对该类物质的整类列管。

A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method with QuEChERS and solid phase extraction(SPE) cleanup was developed for determination of 27 novel fentanyl analogs and metabolites in solid and liquid drugs.The confirmation was achieved with electrospray ionization(ESI) in positive ion mode under multiple reaction monitoring(MRM) mode,and quantified by the external standard method.The standard curves for 27 target compounds were linear in the range of 0.5-50.0 μg/L,with their correlation coefficients(r^2) more than 0.99.The limits of quantitation(LOQ) were 10.0 μg/kg for solid drugs and 10.0 μg/L for liquid drugs,respectively.Recoveries at three spiked levels ranged from 84.8% to 109% with relative standard deviations(RSD) of 0.86%-8.5%.With the advantages of rapidness,simplicity,time-saving,high sensitivity and good stability,the method could be applied in the qualitative and quantitative detection of fentanyl analogs and metabolites in drugs.