郁东，王德军，朱文文，陈田，施致雄
单位
1.山东省职业卫生与职业病防治研究院检验科；2.山东省疾病预防控制中心；3.首都医科大学公共卫生学院
基金项目:国家自然科学基金(21477083)；山东省医药卫生科技发展计划项目(2013WS0159)；首都医科大学校自然科学基金(2016ZR01)；北京市自然科学基金(7122022)
中文摘要:建立了QuEChERS前处理结合气相色谱-质谱快速测定职业工人尿液中8种多溴联苯醚同系物的分析方法。尿液样在氯化钠和无水硫酸镁的脱水与盐析作用下以正己烷-丙酮混合液提取，采用C18去除提取液中的杂质，并采用气相色谱-负化学源质谱法在选择离子监测模式下测定，内标法定量。三至七溴联苯醚在1~100 pg/μL(十溴联苯醚为10~1 000 pg/μL)范围内线性关系良好，相关系数均大于0.999。待测物在3个加标水平下的平均回收率为91.7%~110.2%，相对标准偏差(RSD)小于10%。多溴联苯醚的检出限为0.3~36 pg/mL。该方法简单快速，灵敏度和选择性较高，适合职业工人体内污染物暴露水平监测。
中文关键词:多溴联苯醚 尿液 气相色谱-质谱(GC-MS) 职业工人
Rapid Determination of Polybrominated Diphenyl Ethers in Urine of Occupational Worker Using QuEChERS Coupled to Gas Chromatography-Mass Spectrometry
Abstract:A method for the analysis of polybrominated diphenyl ethers(PBDEs) in urine of occupational worker was developed using QuEChERS(quick，easy，cheap，effective，rugged，safe) pretreatment coupled to gas chromatography-mass spectrometry(GC-MS).Urine sample was extracted with an acetone-hexane mixture by dehydration and salting-out using NaCl and anhydrous MgSO4.The purification was performed with C18 particlet,and GC-MS determination was perfomed under negative chemical ionization(NCI) mode.The calibration curves were linear in the ranges of 10-1 000 pg/μL for BDE-209，and 1-100 pg/μL for the rest of analytes，with correlation coefficients higher than 0.999 .The average recoveries were in the range of 91.7%-110.2% at three spiked levels，with relative standard deviations lower than 10%.The limits of detection(LOD) of PBDEs ranged from 0.3 pg/mL to 36 pg/mL.This method was validated to be simple，sensitive and selective，and was suitable for the exposure accessment of pollutant in occupational workers.
Key Words:polybrominated diphenyl ethers(PBDEs) urine gas chromatography-mass spectrometry(GC-MS) occupational worker
引用本文：郁东，王德军，朱文文，陈田，施致雄.QuEChERS结合气相色谱-质谱法快速测定职业工人尿液中多溴联苯醚[J].分析测试学报,2017,36(5):640-644.
