摘要
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)法测定环境水样中碘代造影剂碘帕醇和碘海醇。样品加入等体积乙腈稀释后离心后,采用PHNOMON Kinetex F5柱(100 mm×3 mm,2.6μm)进行分离,以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱,在电喷雾离子源、正离子模式下,采用多反应检测模式检测,碘海醇和碘帕醇的定量离子对分别为m/z821.8/602.9和m/z777.8/558.8,利用外标法定量。碘海醇在0.01~20μg/L范围内,碘帕醇在0.50~50μg/L范围内,相关系数(r)≥0.9956。地表水和地下水水样中,碘海醇和碘帕醇的回收率为84.1%~109.1%,相对标准偏差为4.1%~9.3%,不同类型水样的基质效应系数在0.88~1.02之间。碘海醇与碘帕醇的检出限(S/N=3)分别为0.004μg/L和0.5μg/L。
A rapid analysis method based on ultra high performance liquid chromatography-tandem mass spectrometer(UPLC-MS/MS) was established for the simultaneous detection of iohexol and iopamidol residues in environmental water samples.Water samples were firstly diluted with equal volume of acetonitrile and then centrifed.The targets were separated with a pentaflurophenyl column using H_(2)O with 0.1% formic acid(V/V) and acetonitrile as mobile phases,and then were introduced into the electrospray ionization(ESI) source for further multiple-reaction monitoring(MRM) in positive mode.Iohexol and iopamidol were quantified with external standard method.The results showed good linearity in the range of 0.01-20 μg/L and 0.5-50 μg/L with the correlation coefficients of 0.9956 and 0.9995 for iohexol and iopamidol,respectively.For ground water samples and surface water samples,the recovery of iohexol and iopamidol ranged from 84.1% to 109.1% and matrix effect coefficient ranged from 0.88-1.02.The limit of detection(LOD,S/N=3) was 0.004 μg/L for iohexol and 0.05 μg/L for iopamidol.
作者
张爽
宋宁慧
范义锋
李旦
ZHANG Shuang;SONG Ninghui;FAN Yifeng;LI Dan(StateKey Laboratory of Food Science and Technology,Nanchang University,Wuxi 214122;Nanjing Institute of Environmental Sciences,Nanjing 210042;Guangzhou Ingenious Laboratory Technology Co.Ltd.,Guangzhou 510535;Wuxi Molecular Bridge Co.Ltd.,Wuxi 214021)
出处
《分析科学学报》
CAS
CSCD
北大核心
2022年第2期197-202,共6页
Journal of Analytical Science
基金
国家重点研发计划(No.2019YFD110303-4)。
关键词
超高效液相色谱-串联质谱
碘海醇
碘帕醇
水样
Ultra-high performance liquid chromatography-tandem mass spectrometer
Iohexol
Iopamidol
Water sample
