在线固相萃取-超高效液相色谱-串联质谱测定饮用水中10种有机磷阻燃剂  

Determination of 10 organophosphorus flame retardants in drinking water by On-line SPE-UPLC-MS/MS

作　　者：郑磊 闵巍 詹铭[1] 赵宜静[1] ZHENG Lei;MIN Wei;ZHAN Ming;ZHAO Yijing(Pudong District Center for Disease Control and Prevention,Shanghai 200136,China)

机构地区：[1]上海市浦东新区疾病预防控制中心,上海200136

出　　处：《公共卫生与预防医学》2023年第2期45-49,共5页Journal of Public Health and Preventive Medicine

基　　金：上海市浦东新区科技发展基金民生科研专项资金(医疗卫生)项目(PKJ2020-Y62);上海市浦东新区卫生系统公共卫生学科建设资助(PWGw2020-04)。

摘　　要：目的建立在线固相萃取-超高效液相色谱-串联质谱(On-line SPE-UPLC-MS/MS)测定饮用水中10种有机磷阻燃剂的方法。方法水样加入内标后,经微孔滤膜过滤后直接进样,采用在线固相萃取-超高效液相色谱-串联质谱(On-line SPE-UPLC-MS/MS)系统进行富集浓缩并测定。样品利用C 8固相萃取柱富集浓缩,利用C 18色谱柱分离待测物,采用乙腈-水-甲酸为流动相梯度洗脱,负离子模式下,多反应监测(MRM)模式检测。结果10种有机磷阻燃剂在一定范围内均有良好的线性关系,线性相关系数(r)>0.990。检出限为0.6~5.5 ng/L,低、中、高3种级别质量浓度的加标回收率分别为64%~106%、83%~104%、85%~99%。结论该方法操作简单,灵敏快速、准确可靠,适用于饮用水中10种有机磷阻燃剂的痕量检测。Objective To establish a method for the determination of 10 organophosphorus flame retardants in drinking water by on-line solid phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry(On-line SPE-UPLC-MS/MS).Methods After adding the internal standard,the water sample was filtered by Millipore filtration,and then concentrated and detected by Online SPE-UPLC-MS/MS.Samples were concentrated by C 8 SPE column and separated by C 18 column with acetonitrile-water-formic acid as the mobile phases gradient elution,and were detected by multiple reaction monitoring(MRM)acquisition under anion mode.Results The 10 organophosphorus flame retardants all displayed good linear relationships within a certain range of concentrations,with the correlation coefficients being more than 0.990.The method detection limits were 0.60-5.50 ng/L,and the spiked recoveries of low,medium and high concentrations were 64%-106%,83%-104%and 85%-99%,respectively.Conclusion The method is simple,sensitive,rapid,accurate and reliable,so it is applicable for the determination of 10 organophosphorus flame retardants in drinking water.

关 键 词：在线固相萃取-超高效液相色谱-串联质谱 有机磷阻燃剂 饮用水 

分 类 号：R123[医药卫生—环境卫生学]