超高效液相色谱-电喷雾串联质谱法同时测定地表水中28种皮质激素  

Simultaneous determination of 28 corticosteroids in surface water by ultra-high performance liquid chromatographyelectrospray tandem mass spectrometry

作　　者：龚剑[1] 林粲源 熊小萍[1] 陈迪云[1] 陈永亨[1] 吴翠琴[1] GONG Jian;LIN Canyuan;XIONG Xiaoping;CHEN Diyun;CHEN Yongheng;WU Cuiqin(School of Environmental Science and Engineering,Guangzhou University,Key Laboratory for Water Quality and Conservation of the Pearl River Delta,Ministry of Education,Guangdong Provincial Key Laboratory of Radionuclides Pollution Control and Resources,Guangzhou 510006,China)

机构地区：[1]广州大学环境科学与工程学院,珠江三角洲水质安全与保护省部共建教育部重点实验室,广东省放射性核素污染控制与资源化重点实验室,广东广州510006

出　　处：《色谱》2018年第11期1158-1166,共9页Chinese Journal of Chromatography

基　　金：国家自然科学基金(41673110);广州市科技计划项目(201607010217);广州市属高校科技计划项目重点项目(1201410747).

摘　　要：建立了同时测定地表水中28种皮质激素的超高效液相色谱-电喷雾串联质谱(UHPLC-ESI-MS/MS)的分析方法。水样经HLB柱固相萃取、C_8反相色谱柱分离,在动态多反应监测(DMRM)模式下采用电喷雾离子化正、负离子模式(ESI±)进行信号采集与测定,内标法定量。结果发现,28种皮质激素在1. 0～100μg/L范围内具有良好的线性关系(R2>0. 99),方法检出限为0. 21～0. 48 ng/L,方法定量限为0. 32～0. 72 ng/L。在5. 0、10、50 ng/L的基质加标水平下,28种目标物的平均回收率为68. 8%～108. 7%,相对标准偏差为0. 1%～8. 1%。该方法灵敏、准确、可靠,将广泛应用于环境中糖/盐皮质激素的痕量监测及其行为、风险研究。A comprehensive analytical method was developed for simultaneous determination of 28 corticosteroids in surface water based on ultra-high performance liquid chromatography-electrospray tandem mass spectrometry(UHPLC-ESI-MS/MS).The solid-phase extraction was performed using hydrophilic-lipophilic balance(HLB)cartridges,and the chromatographic separation was achieved on a reversed-phase C8 column.Qualitative and quantitative analyses were performed in the dynamic multiple reaction monitoring(DMRM)mode using positive and negative electrospray ionization(ESI±).The 28 target compounds were quantified by the internal standard method.Good linear relationships were obtained(R 2>0.99)for the 28 analytes in the concentration range of 1.0-100μg/L.The method limits of detection and quantification were in the range of 0.21-0.48 ng/L and 0.32-0.72 ng/L,respectively.When the matrix spiking levels were at 5.0,10,and 50 ng/L,the average recoveries for the target compounds ranged from 68.6%to 108.7%,and the relative standard deviations(RSDs)were between 0.1%and 8.1%.Because of its high sensitivity,good precision,and reliability,this method can be widely applied to trace monitoring of glucocorticoids and mineral ocorticoids for investigating their behaviors and risks of corticosteroids in the environment.

关 键 词：超高效液相色谱-串联质谱 皮质激素 地表水 

分 类 号：O658[理学—分析化学]