2023年河北大学学报(自然科学版)2023第43卷第2期JournalofHebeiUniversity(NaturalScienceEdition)Vol.43No.2DOI:10.3969/j.issn.10001565.2023.02.008超高效液相色谱-三重四极杆串联质谱法检测全血中常见安眠镇静类药物方雅莉1,马骥2(1.广东医科大学科研平台服务管理中心,广东东莞523000;2.东莞市公安局物证鉴定中心,广东东莞523000)摘要:建立了超高效液相色谱-三重四极杆复合线性离子阱质谱快速筛查确证全血中49种安眠镇静类药物.样品前处理采用固相支撑液液萃取法.色谱条件:色谱柱为WatersC18(2.1mm×50mm,1.7μm),以5mmol/L乙酸铵-(体积分数为0.1%)甲酸水溶液(A),甲醇(B)为流动相,进行梯度洗脱.在0.1~200.0ng/mL内,49种常见药物展现出良好的线性关系(R2>0.99),最高检出限为0.1ng/mL;最高定量限为0.5ng/mL;全血基质中50、100、200ng/mL3个加标水平下回收率为65.9%~109.0%,日内精密度为2.0%~17.6%、日间精密度为2.0%~16.3%.该方法可应用于生物检材中49种常见安眠镇静物质的检测.关键词:安眠镇静类药物;超高效液相色谱串联质谱;全血中图分类号:O657.7文献标志码:A文章编号:10001565(2023)02016308DeterminationofcommonhypnoticandsedutivedrugsinwholebloodbyUPLC-MS/MSFANGYali1,MAJi2(1.ScientificResearchPlatformServiceManagementCenter,GuangdongMedicalUniversity,Dongguan523000,China;2.ForensicScienceCenter,DongguanPublicSecurityDepartment,Dongguan523000,China)Abstract:Ahighthroughputscreeningmethodbasedonultraperformanceliquidchromatogramphy-triplequadrupolecompositelineariontrapmassspectrometry(UPLC-Q-TRAP/MS)wasdevelopedforthesimultaneousandrapidconfirmationof49commonhypnoticandsedutivedrugs.Thepre-treatmentmethodwasbasedonsolid-supportedliquidliquidextraction(SLE).WatersC18chromatographiccolumn(2.1mm×50mm,1.7μm)wasselected,with0.1%(V/V)formicacid,5mmoL/Lammoniumacetateaqueoussolutionandmethanolasmobilephasesforgradientelution.Thecalibrationcurvesshowedgoodlinearityintherangeof0.1~200.0ng/mL,withcorrelationcoefficients(R2)greaterthan0.99forall49analytes.Thelimitsofhighestdetectionandhighestquantificationofthe49compoundswere0.1ng/mLand0.5ng/mL,respectively.Atspikedlevelsof50、100、200ng/mL,recoveries,intra-dayprecisions,andinter-dayprecisionsofthe4...
