液相萃取-气相色谱-质谱法快速分析血清中有机磷酸酯类 三(2,4-二叔丁基苯基)-磷酸酯(AO168O)和 2,4-二叔丁基苯基(2,4DtBP)  

Rapid determination of tris(2,4-di-tert-butylphenyl)-phosphate(AO168O)and 2,4-di-tert-butylphenyl(2,4DtBP)in human serum by liquid phase extraction-gas chromatography-mass spectrometry

作　　者：卢柏灵 蔡利梅 刘思[1,2] 郭丽琼 彭子娟 王晓丽 宋善军[2] 李彭辉 LU Boling;CAI Limei;LIU Si;GUO Liqiong;PENG Zijuan;WANG Xiaoli;SONG Shanjun;LI Penghui(Tianjin University of Technology,Tianjin,300384,China;National Institute of Metrology,Beijing,100029,China;Tianjin University,Tianjin,300072,China)

机构地区：[1]天津理工大学,天津300384 [2]中国计量科学研究院,北京100029 [3]天津大学,天津300072

出　　处：《环境化学》2023年第4期1128-1136,共9页Environmental Chemistry

基　　金：国家自然科学基金(21806158);中国计量科学研究院基本科研业务费(AKY1720);博士后基金(2020M670667);Environmental and Lifestyle in Metabolic Health Throughout Life-Course Trajectories(ELEFANT,No.TmuhMEC2016022);中新天津生态城2019年度科技型中小企业升级专项项目资助.

摘　　要：本研究建立了液相萃取-气相色谱-质谱法快速测定血清中三(2,4-二叔丁基苯基)-磷酸酯(tris(2,4-di-tert-butylphenyl)-phosphate,AO168O)和2,4-二叔丁基苯基(2,4-di-tert-butylphenyl,2,4DtBP).血清样品经乙腈提取,离心分离,浓缩定容后进行仪器分析.采用DB-5MS(30 m×0.25 mm,0.25μm)色谱柱进行分离,多重反应监测模式(MRM)进行测定.结果表明,AO168O在0.8—100 ng·mL^(−1)范围内线性关系良好,2,4DtBP在0.6—100 ng·mL^(−1)范围内线性关系良好,相关系数R 2分别为0.9992和0.9995;方法检出限分别为0.4 ng·mL^(−1)和0.2 ng·mL^(−1);加标回收率分别为103%和95%,相对标准偏差(n=5)分别为8.9%和4.7%.采用本方法对天津市青年人群的66份血清样品进行检测,AO168O的检出率为33%,2,4DtBP的检出率为98%,浓度范围分别为ND(未检出)—492.33 ng·mL^(−1)和ND—21.63 ng·mL^(−1).本研究所建立的方法适用于快速测定血清中的AO168O和2,4DtBP,对进一步评估AO168O和2,4DtBP的人体暴露风险具有重要意义.A liquid phase extraction-gas chromatography-mass spectrometry method was established for rapid determination of tris(2,4-di-tert-butylphenyl)-phosphate(AO168O)and 2,4-ditert-butylphenyl(2,4DtBP)in human serum.The samples were extracted by acetonitrile and the supernatant was centrifuged and concentrated for further instrumental analysis.The separation was performed on a DB-5MS(30 m×0.25 mm,0.25μm)column,and the determination was performed in multiple reaction monitoring mode(MRM).The results showed good linearity for AO168O and 2,4DtBP,in the range of 0.8—100 ng·mL^(−1) and 0.6—100 ng·mL^(−1),respectively.The correlation coefficient of AO168O and 2,4DtBP were 0.9992 and 0.9995,respectively.The limits of detection for AO168O and 2,4DtBP were 0.4 ng·mL^(−1) and 0.2 ng·mL^(−1),respectively.The spiked recoveries(n=5)of AO168O and 2,4DtBP were 103%and 95%,and the relative standard deviations(RSDs)were 8.9%and 4.7%,respectively.The method was applied to the determination of AO168O and 2,4DtBP in 66 serum samples from a young population in Tianjin,China.The detection frequencies of two analytes were 33%and 98%.The concentrations of AO168O and 2,4DtBP ranged from not detected(ND)to 492.33 ng·mL^(−1) and ND to 21.63 ng·mL^(−1),respectively.The method is suitable for rapid determination of AO168O and 2,4DtBP in human serum and is important for further risk assessment of human exposure.

关 键 词：气相色谱-串联质谱 液相萃取 三 (2 4-二叔丁基苯基)-磷酸酯 2 4-二叔丁基苯基 血清 

分 类 号：O657.63[理学—分析化学] R994.6[理学—化学]