加速溶剂萃取-凝胶渗透色谱-气相色谱-串联质谱法测定鱼类中7种新型有机污染物

Determination of 7 kinds of emerging organic pollutants in fish by accelerated solvent extraction-gel permeation chromatography-gas chromatography-tandem mass spectrometry

中文关键词:  加速溶剂萃取  凝胶渗透色谱法  气相色谱-串联质谱法  鱼类  卤代咔唑

英文关键词:accelerated solvent extraction  gel permeation chromatography  gas chromatography-tandem mass spectrometry  fish  polyhalogenated carbazoles

中文摘要:

      目的 建立加速溶剂萃取-凝胶渗透色谱-气相色谱-串联质谱法同时测定鱼类中7种新型有机污染物(咔唑和卤代咔唑类化合物)的分析方法。方法 样品与硅藻土研磨混匀后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1 mL丙酮复溶。目标化合物采用多反应监测(multiple reaction monitoring, MRM)模式分析, 外标法进行定量。结果 咔唑、3-氯咔唑、3-溴咔唑和3,6-二氯咔唑在0.5~50.0 μg/kg范围内线性关系良好, 相关系数r>0.997; 3,6-二溴咔唑、2,7-二溴咔唑和1,3,6,8-四溴咔唑在1.0~100.0 μg/kg范围内线性关系良好, 相关系数r>0.998。定量限(limits of quantification, LOQs)在0.50~1.00 μg/kg之间, 在各目标物的1 LOQs、2 LOQs和10 LOQs 3个加标水平下, 7种咔唑和卤代咔唑类化合物的平均回收率为87.22%~107.27%, 相对标准偏差(relative standard deviations, RSDs)为2.70%~8.17% (n=6)。结论 该方法自动化程度高、灵敏度高、稳定性好, 适用于鱼类中7种咔唑和卤代咔唑类化合物的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 7 kinds of emerging organic pollutants in fish by accelerated solvent extraction-gel permeation chromatography-gas chromatography-tandem mass spectrometry. Methods The samples were mixed and ground with diatomite and extracted by accelerated solvent extraction, purified by gel permeation chromatography, blow to nearly dryness by nitrogen, and redissolved in 1 mL acetone. They were analyzed in the multiple reaction monitoring (MRM) mode and quantified by external standard method. Results The carbazole, 3-chlorocarbazole, 3-bromo carbazole and 3,6-dichlorocarbazole showed good linear relationships in the range of 0.5?50.0 μg/kg with the correlation coefficient r>0.997; the 3,6-dibromo carbazole, 2,7-dibromo carbazole and 1,3,6,8-tetrabromo carbazole showed good linear relationships in the range of 1.0?100.0 μg/kg with the correlation coefficient r>0.998. The limits of quantification (LOQs) were 0.50?1.00 μg/kg, and the average recoveries of 7 kinds of carbazole and polyhalogenated carbazoles were 87.22%?107.27% at the 3 kinds of spike levels of LOQs, 2-fold LOQs and 10-fold LOQs. The relative standard deviations (RSDs) were 2.70%?8.17% (n=6). Conclusion This method is highly automatic, process shighly sensitive, reasonably stable, and can be used for the determining of 7 kinds of carbazole and polyhalogenated carbazoles in fish.