直接进样-LC-MS/MS测定水中16种有机磷酸酯类化合物  

Simultaneous determination of 16 organophosphates in waters by direct injection LC-MS/MS

作　　者：刘殿甲 吴宇峰 张静 左明 王效国 王洪乾 张肇元 郭栋 LIU Dianjia;WU Yufeng;ZHANG Jing;ZUO Ming;WANG Xiaoguo;WANG Hongqian;ZHANG Zhaoyuan;GUO Dong(Tianjin Eco-Environmental Monitoring Center,Tianjin,300191,China;Tianjin-Tianbinruicheng Environmental Technology and Engineering Co.,Ltd.,Tianjin,300190,China)

机构地区：[1]天津市生态环境监测中心,天津300191 [2]天津天滨瑞成环境技术工程有限公司,天津300190

出　　处：《环境化学》2023年第4期1165-1175,共11页Environmental Chemistry

摘　　要：本文通过对空白污染消除和样品前处理方法优化,建立了直接进样-高效液相色谱串联质谱测定水中有机磷酸酯类化合物(OPEs)的检测方法.通过液相色谱流路中安装捕集柱、清洗进样瓶、以玻璃注射器代替移液枪、过滤用PTFE滤膜可以消除相应空白污染;通过水样过滤前加入1倍体积甲醇可以减少滤膜对高脂溶性OPEs的截留,物质回收率提高至80%以上.方法优化后,16种OPEs标准曲线R 2均大于0.995,检出限在1.40×10^(−3)—0.04μg·L^(−1).实验室空白水样低、中、高浓度的物质加标回收率和相对标准偏差(n=6)分别在70.4%—110%和1.8%—15.4%;污水处理厂出水水样的物质加标回收率和相对标准偏差(n=6)分别为70.5%—119%和2.6%—25.8%.因此,优化的方法具有较高的精密度和准确度,可以满足直接进样法检测OPEs的需求.A method was developed for simultaneous determination of 16 organophosphates(OPEs)in waters by liquid chromatography tandem quadrupole mass spectrometry with direct injection.Sources and solution of whole process blank pollution and the optimization of pretreatment method were studied.Pollutions can be eliminated by installing catcher column,washing sample vials,replacing pipette tip with glass syringe,and using PTFE membrane during the filtration process.In order to decrease the retention of OPEs with high fat solubility on membrane,the same volume of methanol was added to samples before filtering.The results showed that recoveries of OPEs were improved to over 80%using the optimizing method.And the R 2 of calibration curve was greater than 0.995,the detection limits of OPEs in water ranged from 1.40×10^(−3)μg·L^(−1) to 0.04μg·L^(−1).The recoveries and the relative standard deviations(RSDs)(n=6)for low,medium and high levels spiking blanks ranged from 70.4%to 110%and from 1.8%to 15.4%,respectively.The recoveries of spiking waste water ranged from 70.5%to 119%with RSDs(n=6)of 2.6%—25.8%.All the results above showed that the method is sensitive,accurate and reliable,and it can meet the requirements for the determination of OPEs in water by direct injection.

关 键 词：有机磷酸酯类物质 (OPEs) 直接进样 高效液相色谱串联质谱法 背景污染消除 

分 类 号：X832[环境科学与工程—环境工程]