| 羧基化多壁碳纳米管分散固相萃取/气相色谱-质谱法测定茶青中18种多氯联苯 |
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| 基金项目:国家农业基础性长期性科技项目（ZX10S1108）；省部共建国家重点实验室培育基地“江苏省食品质量安全重点实验室”开放课题（201603）；苏州市科技计划项目（SNG201622,SNG201644,SNG2018098） |
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| 中文摘要:建立了超声提取、分散固相萃取净化结合气相色谱-质谱（GC-MS）同时检测茶青中18种多氯联苯（PCBs）的方法。样品经正己烷-丙酮（1∶1,体积比）超声提取，通过甲苯溶剂置换后，用羧基化多壁碳纳米管（MWCNTs-COOH）和N 丙基乙二胺（PSA）吸附剂净化，在GC-MS选择离子监测模式下进行测定，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。优化了气相色谱-质谱条件，考察了提取溶剂及吸附剂种类和用量、提取时间和净化时间对分析结果的影响。在最优实验条件下，18种PCBs在5～500 μg/kg范围内线性关系良好，相关系数不低于0.999 8；在5、10、100 μg/kg加标水平下，平均回收率为92.3%～111%，相对标准偏差（n=6）为1.2%～7.9%；方法检出限为0.5～1.4 μg/kg，定量下限均为5 μg/kg。该法操作简单、快速准确、灵敏度高、样品净化效果好，可用于茶青中18种PCBs的同时检测。 |
| 中文关键词:羧基化多壁碳纳米管 分散固相萃取 气相色谱-质谱（GC-MS） 茶青 多氯联苯（PCBs） |
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| Determination of 18 Polychlorinated Biphenyls in Fresh Tea Leaves by Gas Chromatography-Mass Spectrometry with Carboxylated Multi walled Carbon Nanotubes as Dispersive Solid Phase Extraction Sorbent |
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| Abstract:A gas chromatograph-mass spectrometric（GC-MS） method based on ultrasound assisted extraction and dispersive solid phase extraction was developed for the simultaneous determination of 18 polychlorinated biphenyls（PCBs） in fresh tea leaves.The samples were extracted using a mixture of hexane-acetone（1∶1,by volume） by ultrasonic extraction,and cleaned up with the mixed sorbents of carboxylated multi walled carbon nanotubes（MWCNTs-COOH） and primary secondary amine（PSA） after replacing hexane-acetone by toluene,then detected by GC-MS under selected ion monitoring mode.The PCBs were qualitatively confirmed by retention time and relative abundance ratio of characteristic ions,and quantified by the external standard method with matrix matched standards solution.The chromatographic and MS parameters influencing separation and sensitivity were optimized,and several important factors affecting extraction and purification efficiency such as type and volume of extraction solvent,extraction time,type and amount of cleanup sorbent and cleanup time were investigated.Under the optimum conditions,satisfactory linear relationships for the analytes were observed in the concentration range of 5-500 μg/kg with correlation coefficients not less than 0.999 8.The recoveries for 18 PCBs in fresh tea leaves at spiked levels of 5,10 and 100 μg/kg were in the range of 92.3%-111% with relative standard deviations（n=6） of 1.2%-7.9%.The limits of detection and the limits of quantitation for PCBs were 0.5-1.4 μg/kg and 5 μg/kg,respectively.The method was simple,rapid,accurate,sensitive and effective in purification,and was suitable for the determination of 18 PCBs in fresh tea leaves. |
| Key Words:carboxylated multi walled carbon nanotubes dispersive solid phase extraction gas chromatography-mass spectrometry（GC-MS） fresh tea leaves polychlorinated biphenyls（PCBs） |
| 引用本文：刘腾飞，杨代凤，章雪明，范君，梁凤玲，钱辉.羧基化多壁碳纳米管分散固相萃取/气相色谱-质谱法测定茶青中18种多氯联苯[J].分析测试学报,2018,37(12):1405-1411. |
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