摘要
建立了测定土壤中18种多氯联苯的气相色谱/质谱分析方法。样品经丙酮-正己烷(1∶1,V/V)超声提取,通过甲苯置换后,以羧基化多壁碳纳米管(MWCNTs-COOH)为吸附剂,用分散固相萃取净化,采用气相色谱/质谱法,在选择离子监测模式下检测,以保留时间和特征离子丰度比定性,基质匹配标准溶液外标法定量。结果表明,MWCNTs-COOH用于土壤样品净化效果好,0.02gMWCNTs-COOH能够有效除去基质中杂质对测定结果的影响。18种待测物在5~500μg/kg范围内线性关系良好,相关系数不低于0.9998;方法的加标回收率为90.1%~111.7%,相对标准偏差(RSD,n=6)为1.2%~15.3%,检出限为0.5~1.4μg/kg,定量限为1.6~4.4μg/kg。该方法操作简便、准确度好、溶剂用量少、净化效果好,可以用于土壤中18种多氯联苯的同时测定。
A gas chromatograph/mass spectrometry(GC/MS)method was developed for the determination of 18 polychlorinated biphenyls(PCBs)in soil.The PCBs were extracted using a mixture of acetone-hexane(1∶1,by volume),and cleaned up with carboxylated multi-walled carbon nanotubes(MWCNTs-COOH)as dispersive solid phase extraction(DSPE)sorbent after replacing hexane-acetone by toluene,then detected by GC/MS under selected ion monitoring mode.Identification was achieved by retention time and relative abundance ratio of characteristic ions,and quantification was done by the external standard method with matrix-matched standards solution.MWCNTs-COOH were proved to be a promising DSPE sorbent with excellent cleanup efficiency to soil martix,and the optimal amount of 0.02 g MWCNTs-COOH was suitable for cleaning up soil samples.Satisfactory linear relationships for the analytes were observed in the concentration range of 5-500μg/kg with correlation coefficients no less than 0.9998.The average recoveries for 18 PCBs in soil samples at spiked levels of 5,10 and 100μg/kg ranged from 90.1%to 111.7%with relative standard deviations(n=6)between 1.2%and 15.3%.The limits of detection and the limits of quantification for PCBs were 0.5-1.4μg/kg and 1.6-4.4μg/kg,respectively.This method is simple,accurate,solvent saving and effective in purification,and provides a useful assay to simultaneously determine 18 PCBs in soil.
作者
刘腾飞
杨代凤
范君
毛健
孙灵湘
董明辉
LIU Teng-fei;YANG Dai-feng;FAN Jun;MAO Jian;SUN Ling-xiang;DONG Ming-hui(Jiangsu Taihu Area Institute of Agricultural Sciences,Suzhou 215155)
出处
《分析科学学报》
CAS
CSCD
北大核心
2019年第4期467-473,共7页
Journal of Analytical Science
基金
国家农业基础性长期性科技项目(No.ZX10S1108)
江苏省食品质量安全重点实验室开放课题(No.201603)
苏州市科技计划(No.SNG201622,SNG201644,SNG2018098)
关键词
多氯联苯
土壤
羧基化多壁碳纳米管
分散固相萃取
气相色谱/质谱
Polychlorinated biphenyls
Soil
Carboxylated multi-walled carbon nanotubes
Dispersive solid-phase extraction
Gas chromatography/mass spectrometry
