超声波提取–气相色谱–质谱法测定脱水污泥中的多氯联苯

Determination of PCBs in dewatering sludge by UE–GC–MS

采用超声波提取,气相色谱–质谱联用法检测,建立了脱水污泥中18种多氯联苯的测定方法。污泥样品以二氯甲烷-正己烷(体积比为1∶1)为提取剂,用超声波提取20 min,在优化的仪器条件下,其中18种多氯联苯的质量浓度在0.05～100μg/mL范围内与色谱峰面积均呈良好的线性关系(r≥0.999 0)。方法的检出限为0.16～0.97μg/L,加标回收率为84.0%～117.0%,测定结果的相对标准偏差小于4.5%(n=6)。该方法样品前处理简单,重现性好,检出限低,准确度高,适用于污水处理厂脱水污泥中18种多氯联苯的测定。

A method of ultrasonic extraction combined gas chromatography-mass spectrometry( UE-GC-MS ) was established to determine 18 kinds of PCBs in dewatering sludge from sewage treatment plant.Dichloromethane-hexmethane with volume ratio of 1∶1 as the extracting agent,the sludge sample was extracted for 20 min by ultrasonic.Under optimizing experimental conditions,the mass concentration of 18 PCBs was linear with the chromatographic peak area in the range of 0.05-100μg/mL with the correlation coefficients not less than 0.9990.The detection limits were 0.16-0.97μg/L.The spiked recoveries ranged from 84.0% to 117.0%,and the relative standard deviations of detection results were less than 4.5%(n=6).This method is simple in sample pretreatment with good reproducibility and high accuracy,it is suitable for the determination of 18 kinds of PCBs in dewatering sludge from sewage treatment plants.