加速溶剂萃取—凝胶渗透色谱净化—气相色谱—串联质谱法测定海洋沉积物中9种咔唑和卤代咔唑  

Determination of 9 kinds of carbazole and polyhalogenated carbazoles in marine sediments by accelerated solvent extraction-gel permeation chromatography purification-gas chromatography-tandem mass spectrometry

作　　者：唐雷鸣 蒋玲波 陈翔 高卓瑶 邓招超 王萍亚 倪鲁波 陆羚子 戴意飞 TANG Leiming;JIANG Lingbo;CHEN Xiang;GAO Zhuoyao;DENG Zhaochao;WANG Pingya;NI Lubo;LU Lingzi;DAI Yifei(Zhoushan Institute for Food and Drug Control,Zhoushan Zhejiang 316012;College of Food and Pharmacy,Zhejiang Ocean University,Zhoushan Zhejiang 316000;College of Marine Science,Zhejiang University,Zhoushan Zhejiang 316000)

机构地区：[1]舟山市食品药品检验检测研究院,浙江舟山316012 [2]浙江海洋大学食品与药学学院,浙江舟山316000 [3]浙江大学海洋学院,浙江舟山316000

出　　处：《环境污染与防治》2023年第6期810-816,共7页Environmental Pollution & Control

基　　金：浙江省舟山市公益类科技项目(No.2022C31071)。

摘　　要：建立高效的海洋沉积物样品前处理方法及高灵敏度的气相色谱(GC)—串联质谱(MS/MS)条件精准测定海洋沉积物中9种咔唑(CZ)及卤代咔唑(PHCZs)。冷冻干燥后的海洋沉积物样品经加速溶剂萃取仪提取,使用凝胶渗透色谱法净化并氮吹至近干,用丙酮复溶后采用GC—MS/MS进行检测,外标法定量。结果表明:9种目标物在0.10~10.00μg/kg或0.20~10.00μg/kg内线性关系良好,相关系数大于0.996,该方法定量限为0.10~0.20μg/kg。在1倍、3倍、10倍定量限的加标水平下,9种CZ及PHCZs的回收率为83.5%~115.0%,相对标准偏差为3.43%~9.77%。该方法具有操作步骤简单、自动化程度高、灵敏度高、定性定量准确的优点,满足海洋沉积物中9种CZ及PHCZs的检测需求。This study aims to establish an efficient sample pre-treatment method and highly sensitive gas chromatography(GC)-tandem mass spectrometry(MS/MS)conditions for the accurate determination of 9 kinds of carbazole(CZ)and polyhalogenated carbazoles(PHCZs)in marine sediments.The freeze-dried sediment samples were extracted by accelerated solvent extraction,purified by gel permeation chromatography and then dried in mild nitrogen flow.After resolubilization with acetone,the samples were analyzed by GC-MS/MS and quantified by external standards.The results showed that the standard curves for CZ and different PHCZs were good in the concentration range of 0.10-10.00μg/kg or 0.20-10.00μg/kg with correlation coefficient was greater than 0.996.The limits of quantification of the method were 0.10-0.20μg/kg.The recoveries of CZ and PHCZs were 83.5%-115.0%under different spiking levels of 1-fold limits of quantification(LOQ),2-fold LOQ and 10-fold LOQ.The relative standard deviations(RSDs)were 3.43%-9.77%.This method had the advantages of simple operation steps,higher automation and sensitivity,accurate characterization and quantification,which could meet the detection requirements of these organic pollutants in marine sediments.

关 键 词：咔唑及卤代咔唑 海洋沉积物 萃取 净化 气相色谱—串联质谱法 

分 类 号：X834[环境科学与工程—环境工程] O657.63[理学—分析化学]