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

Rapid Determination of Polybrominated Diphenyl Ethers in Urine of Occupational Worker Using QuEChERS Coupled to Gas Chromatography-Mass Spectrometry

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/m L。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。

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 NaC1 and anhydrous Mg- SO4. 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.