超高效液相色谱-串联质谱法同时测定环境水体中3种典型“三高”药物残留  

Simultaneous determination of three typical pharmaceuticals for hypertension,hyperglycemia and hyperglycemia in environmental water by UHPLC-MS/MS.

作　　者：陈泽雄 周志洪 巫陪山 马艳芳 Chen Zexiong;Zhou Zhihong;Wu Peishan;Ma Yanfang(Guangzhou Environmental Monitoring Center,Guangzhou 510030,China;Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,China National Analytical Center,Guangzhou 510070,China)

机构地区：[1]广州市环境监测中心站,广州510030 [2]广东省科学院,中国广州分析测试中心,广东省化学危害应急检测技术重点实验室,广州510070

出　　处：《分析仪器》2020年第4期55-62,共8页Analytical Instrumentation

摘　　要：建立了超高效液相色谱-三重四级杆串联质谱(UHPLC-MS/MS)同时测定地表水和污水中3种典型“三高”药物硝苯地平、格列吡嗪和吉非罗齐的分析方法。水样采用Oasis HLB小柱,通过固相萃取方式进行富集、净化,经甲醇/二氯甲烷/乙酸乙酯洗脱后,UPLC-MS/MS进行检测。硝苯地平、格列吡嗪和吉非罗齐在标准曲线溶液中的线性相关系数r 2分别为0.9989、0.9996和0.9998。对于地表水样品,3种目标药物的回收率范围分别为95%~103%、111%~126%和91%~98%,检测限(MQLs,S/N>10)范围为0.13 ng/L^0.79 ng/L,基质效应范围为-3.2%~13%;对于污水样品,3种目标药物的回收率范围分别为71%~80%、87%~113%和105%~112%,MQLs范围为3.35 ng/L^6.32 ng/L,基质效应范围为-14%~19%。方法应用于环境污水样品,检测出硝苯地平浓度为8.7 ng/L。本方法灵敏可靠,可用于环境水体中典型“三高”药物的多残留筛查与痕量检测。The target pharmaceuticals in water sample were concentrated and purified by solid phase extraction with Oasis HLB cartridge,eluted with methanol/dichloromethane/ethyl acetate,and then determined by UHPLC-MS/MS.The linear correlation coefficients r 2 of nifedipine,glipizide and gemfibrozil in standard solution were 0.9989,0.9996 and 0.9998,respectively.For the surface water samples,the spiking recoveries for the 3 targets were in the range of 95%-103%,111%-126%and 91%-98%,the detection limits(MQLs,S/N>10)ranged in 0.13 ng/L-0.79 ng/L,and the matrix effects ranged from-3.2%to 13%;for the wastewater samples,the spiking recoveries for the 3 targets were in the range of 71%-80%,87%-113%and 105%-112%,the detection limits(MQLs,S/N>10)ranged in 3.35 ng/L-6.32 ng/L,and the matrix effects ranged from-14%to 19%.The concentration of nifedipine in wastewater samples was 8.7 ng/L.The proposed method is sensitive and reliable,which can be used for multi-residue screening and trace detection of these pharmaceuticals.

关 键 词：硝苯地平 格列吡嗪 吉非罗齐 多残留筛查 痕量分析 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]