GC-MS/MS法测定沉积物和生物样品中邻苯二甲酸酯  

Determination of phthalate esters in sediments and biological samples by GC-MS/MS

作　　者：时衍伟 王刘勇 张蓉蓉[1] 张泽明 孙爱丽[1] 史西志[1] SHI Yanwei;WANG Liuyong;ZHANG Rongrong;ZHANG Zeming;SUN Aili;SHI Xizhi(School of Marine Sciences,Ningbo University,Ningbo 315823;College of Food and Pharmaceutical Sciences,Ningbo University,Ningbo 315823)

机构地区：[1]宁波大学海洋学院,宁波315823 [2]宁波大学食品与药学学院,宁波315823

出　　处：《分析试验室》2022年第2期141-146,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(31372572);浙江省公益技术研究计划(LGF21C190001);宁波市公益性计划(202002N3066)项目资助。

摘　　要：采用固相萃取(SPE)和QuEChERS技术结合气相色谱-串联质谱(GC-MS/MS)技术,建立了养殖海域沉积物和生物样品中16种邻苯二甲酸酯(PAEs)定量分析方法。沉积物样品以二氯甲烷为提取溶剂,经PSA-Silica固相萃取柱净化,生物样品以乙腈为提取溶剂,经150.0 mg N-丙基乙二胺(PSA)、150.0 mg C18和150.0 mg石墨化碳黑(GCB)净化,在多反应监测模式(MRM)下进行定量分析。结果表明,16种PAEs在质量浓度0.5~300μg/L范围内具有较好的线性相关性(R^(2)>0.9990);沉积物样品中PAEs检出限(LODs)在0.10~1.54μg/kg之间,在10.0,20.0,50.0μg/L 3个添加浓度下的平均回收率为70.1%~110.2%,相对标准偏差(RSD)为2.9%~7.9%;生物样品中PAEs的LODs在0.23~0.96μg/kg范围内,在10.0,20.0,50.0μg/L 3个添加浓度下的平均回收率为71.8%~107.4%,RSD为2.6%~9.1%。方法适用于海洋环境中沉积物和生物中PAEs残留的监测。A precise quantitative analysis method for phthalate esters(PAEs)detection in sediments and biological samples was established using solid phase extraction(SPE)and QuECHERS combined with GC-MS/MS.The sediment samples were extracted with dichloromethane and purified using N-propyl ethanediamine(PSA)-Silica SPE column.The biological samples were extracted with acetonitrile and purified with 150.0 mg PSA,150.0 mg C18 and 150.0 mg graphitized carbon black(GCB).The quantitative analysis was carried out under multi-reaction monitoring mode(MRM).The results showed that linear correlation 16 PAEs was good in the concentration range of 0.5-300μg/L(R^(2)>0.9990).The limits of detection(LODs)of sediment samples were in the range of 0.10-1.54μg/kg,and the average recoveries were 70.1%-110.2%with relative standard deviations(RSDs)of 2.9%-7.9%at three adding concentrations of 10.0,20.0 and 50.0μg/L.For biological samples,LODs ranged from 0.23 to 0.96μg/kg,and the average recoveries were between 71.8%and 107.4%,with RSDs in the range of 2.6%-9.1%.The method is suitable for the monitoring of PAEs in sediments and organisms in marine environment.

关 键 词：GC-MS/MS 邻苯二甲酸酯 固相萃取 QUECHERS 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]