高效液相色谱-串联质谱法测定儿童和成人尿液中双酚A、四溴双酚A和辛基酚  

Determination of Bisphenol A,Tetrabromobisphenol A and 4-TertOctylphenol in Child and Adult Urine Samples Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张圣虎[1] 张易曦 吉贵祥[1] 徐怀洲 刘济宁[1] 石利利[1] 

机构地区：[1]环境保护部南京环境科学研究所,南京210042 [2]贵州大学资源与环境工程学院,贵阳550025

出　　处：《分析化学》2016年第1期19-24,共6页Chinese Journal of Analytical Chemistry

基　　金：国家高技术研究发展计划(863计划)资助项目(No.2013AA06A308)~~

摘　　要：采用高效液相色谱—串联质谱法定量检测人体尿液中痕量双酚A、四溴双酚A和辛基酚。将解冻后的尿样酶解经液液萃取、旋蒸至干,甲醇定容后分析。3种目标物质在0.2-50μg/L质量浓度范围内线性关系良好相关系数均大于0.99定量限（LOQ）在0.05-0.27μg/L之间。在5,10和50μg/L加标水平下平均回收率为85.7%-118.6%相对标准偏差RSD（n=3）为4.1%-10.5%。20组儿童与成人的尿样结果表明,尿样中均检出3种目标物,其中,四溴双酚A和辛基酚在儿童及成人尿样中的暴露浓度基本相同,但是双酚A的暴露水平具有显著性差异（儿童〉成人）。A method using high performance liquid chromatography（HPLC） coupled with tandem mass spectrometry for quantitative determination of bisphenol A（BPA）,tetrabromobisphenol A（TBBPA） and 4-tert-octylphenol（OP） in urine samples of children and adults was developed.The frozen urinary samples were unfrozen at room temperature,extracted by liquid-liquid extraction,evaporated to dryness,and dissolved by methanol so as to be analyzed by LC-MS/MS.The calibration curves for the determination of the three target compounds were linear in the concentration range of 0.2-50 μg/L,correlation coefficients（R） were greater than 0.99,and the quantitative limits（LOQ） were 0.05- 0.27 μg/L.The recoveries of different concentration levels（5,10 and 50 μg/L） were in the range of 85.7%-118.6%and the relative standard deviation（RSD） was 4.1%-10.5%.This method was successfully applied to the determination of BPA,TBBPA and OP in urine samples from 20 groups of children and adults.The results showed that exposure concentrations of TBBPA and OP in urine samples of children and adults were basically same,but exposure levels of BPA had significant difference（children adults（Father or Mother））.

关 键 词：双酚A 四溴双酚A 辛基酚 高效液相色谱-串联质谱法 儿童 成人 尿液 

分 类 号：O657.63[理学—分析化学] R446.12[理学—化学]