固相萃取-气相色谱-串联质谱法测定淡水鱼鱼肉中的五氯酚

Determination of pentachlorophenol in freshwater fish by solid phase extraction-gas chromatography coupled with triple quadrupole mass spectrometry

目的建立采用固相萃取-气相色谱-串联质谱联用为基础的淡水鱼鱼肉中五氯酚的测定方法。方法淡水鱼鱼肉经粉碎后,液液萃取,MAX柱净化,乙酸酐-吡啶溶液衍生成五氯苯乙酸酯,气相色谱-串联质谱仪进行定性和定量分析。结果在1、5、20μg/kg 3个水平下的回收率范围为85.6%~98.4%,相对标准偏差小于10%,方法的定量限为0.85μg/kg(S/N=10),检出限为0.26μg/kg(S/N=3)。结论该方法具有良好的回收率及稳定性,适用淡水鱼鱼肉中五氯酚的测定。

Objective To establish a method for the determination of pentachlorophenol in freshwater fish by gas chromatography coupled with triple quadrupole mass spectrometry. Methods Freshwater fish samples were cleaned up by solid phase extraction, and the elution was dried by N2 and derivatized with acetic anhydride. The derivative was analyzed by gas chromatography coupled with triple quadnlpole mass spectrometry using internal standard method. Results The recoveries at 3 spiked levels of 1,5 and 20 μg/kg were ranged from 85.6% to 98.4%. The relative standard deviations were less than 10%. The limit of quantification was 0.85 μg/kg （S/N=IO）, and the limit of detection was 0.26 μg/kg （S/N=3）. Conclusion This method has good recovery and stability, which is suitable for the determination of pentachlorophenol in freshwater fish.