摘要
建立了超高效液相色谱-串联质谱测定人体尿液中双酚A(BPA)、双酚F(BPF)、四氯双酚A(TCBPA)、四溴双酚A(TBBPA)、壬基酚(NP)、4-正辛基苯酚(4-n-OP)的检测方法。尿液样品通过酶解和固相萃取法进行前处理,采用Acquity UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,负离子电喷雾多反应监测模式检测,同位素内标法定量。6种待测物在0.5~50μg/L范围内线性关系良好,相关系数均大于0.995,检出限为0.05~0.60μg/L,定量下限为0.17~2.00μg/L,2、10、50μg/L加标水平下的回收率为81.4%~112%,相对标准偏差(RSD,n=6)为6.8%~30%。应用此方法测定160份人体尿液样品,双酚A的检出率为93.8%,检出范围为0.24~29.54μg/L,其余目标物未检出。该方法操作简便、重现性好、定量准确,适用于人体尿液中双酚类及烷基酚类物质的测定。
An ultra high performance liquid chromatography-tandem mass spectrometry with solid phase extraction was developed for the determination of bisphenol A(BPA),bisphenol F(BPF),tetrachlorobisphenol A(TCBPA),tetrabromobisphenol A(TBBPA),4-nonylphenol(NP),4-octylphenol(4-n-OP) in human urine.Human urine sample was purified by solid phase extraction after glucuronidase,then separated on an Acquity UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm).The 6 analytes were determined in negative electrospray(ESI-) under multiple reaction monitoring(MRM) mode,and quantified by isotope-labeled internal standard method.There were good linear relationships for 6 analytes in the range of 0.5-50 μg/L with their correlation coefficients larger than 0.995.The limits of detection and the limits of quantitation were in the ranges of 0.05-0.60 μg/L and 0.17-2.00 μg/L,respectively.Recoveries at three spiked levels of 2,10 and 50 μg/L ranged from 81.4% to 112% with relative standard deviations(RSD) of 6.8%-30%.The method was utilized in the determination of 160 human urine samples with a detection rate of 93.8% for BPA in the range of 0.24-29.54 μg/L,and other substances were not detected.With the advantages of convenient operation,good accuracy and stability,this method is suitable for the determination of bisphenols and alkylphenols in human urine.
作者
张卓娜
朱英
林少彬
胡小键
杨艳伟
ZHANG Zhuo-na;ZHU Ying;LIN Shao-bin;HU Xiao-jian;YANG Yan-wei(National Institute of Environmental Health,Chinese Center for Disease Control and Prevention,Beijing 100021,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第3期371-376,共6页
Journal of Instrumental Analysis
关键词
双酚
烷基酚
尿液
超高效液相色谱-串联质谱
固相萃取(SPE)
bisphenols
alkylphenols
urine
ultra high performance liquid chromatography-tandem mass spectrometry
solid phase extraction(SPE)