超声提取-气相色谱串联质谱法测定大气颗粒物PM_(2.5)中18种多氯联苯  

Determination of 18 polychlorinated biphenyls in atmospheric particulate matter PM_(2.5)by ultrasonic extraction coupled with GC-MS/MS

作　　者：李虹霖 秦忠雪[1] 袁悦 雍莉[1] LI Honglin;QIN Zhongxue;YUAN Yue;YONG Li(Sichuan Center for Disease Control and Prevention,Chengdu 610041,Sichuan Province,China)

机构地区：[1]四川省疾病预防控制中心,成都610041

出　　处：《预防医学情报杂志》2025年第1期131-137,144,共8页Journal of Preventive Medicine Information

摘　　要：目的建立超声提取-气相色谱串联质谱法(GC-MS/MS)测定PM_(2.5)中18种多氯联苯的方法,提高空气PM_(2.5)中18种多氯联苯检测效率。方法用PM_(2.5)采样器,以玻璃纤维滤纸为滤料采集空气样品。采样后的玻璃纤维滤膜经正己烷-二氯甲烷(1∶1,v/v)超声提取20 min,氮吹后用正己烷定容,最后注入GC-MS/MS检测分析,外标法定量。结果经正己烷-二氯甲烷(1∶1,v/v)超声提取20 min,18种多氯联苯平均回收率达70%以上。GC-MS/MS方法在0.5~20 ng/ml范围内线性良好,加标回收率为87.7%~119.2%,方法检出限为0.087~0.202 pg/m^(3),相对标准偏差为0.51%~9.39%。结论该样品前处理方法简单高效,仪器方法灵敏准确,可满足PM_(2.5)样品中18种多氯联苯的痕量分析要求。Objective To establish a method for the determination of 18 polychlorinated biphenyls(PCBs)in PM_(2.5)by ultrasonic extraction and gas chromatography tandem mass spectrometry(GC-MS/MS),and to improve the detection efficiency of these 18 PCBs in PM_(2.5)in the air.Methods Atmospheric particulates were collected on fiberglass filter paper as filter material by PM_(2.5)sampler.The sampled glass fiber filter membrane was extracted by n-hexane-dichloromethane(1∶1,v/v)ultrasound for 20 minutes.The extracting solution was concentrated by dryness under nitrogen,reconstituted with n-hexane and finally injected into GC-MS/MS for detection and analysis.Quantitative analysis was completed by external standard method.Results The average recovery of 18 PCBs was over 70%after 20 minutes of ultrasonic extraction of n-hexane-dichloromethane(1∶1,v/v).The GC-MS/MS method had good linearity in the range of 0.5-20 ng/mL.The recoveries were ranged from 87.7%to 119.2%.The method detection limits were 0.087 to 0.202 pg/m^(3).And the relative standard derivation was between 0.51%and 9.39%.Conclusions The sample pretreatment method was simple and efficient,and the instrumental method was sensitive and accurate,which can meet the requirements of trace analysis of 18 PCBs in PM_(2.5)samples.

关 键 词：多氯联苯 持久性有机污染物 PM_(2.5) 超声提取 GC-MS/MS 

分 类 号：X831[环境科学与工程—环境工程] O657.63[理学—分析化学]