固相萃取-气相色谱-质谱法同时测定海参中扑草净和甲氰菊酯残留量

Determination of prometryn and fenpropathrin residue in Apostichopus japonicus by solid-phase extraction-gas chromatography-mass spectrometry

中文关键词:  海参  扑草净  甲氰菊酯  固相萃取  气相色谱-质谱联用仪

英文关键词:Apostichopus japonicus  prometryn  fenpropathrin  solid-phase extraction  gas chromatography-mass spectrometry

中文摘要:

      目的 建立固相萃取-气相色谱-质谱法(solid-phase extraction-gas chromatography-mass spectrometry, SPE-GC/MS)同时检测海参中扑草净和甲氰菊酯残留量的方法。方法 海参经乙腈提取, Cleanert Florisil固相萃取柱萃取净化, 正己烷定容。使用基质溶液配制标准品, 采用选择离子检测模式检测。同时比较了不同提取溶剂类型、提取溶剂用量、固相萃取柱、洗脱液比例对提取效果的影响。结果 扑草净添加水平在5~20 μg/kg时, 回收率在86.3%~106.0%之间, 相对标准差在5.4%~11.6%之间, 定量限为5 μg/kg。甲氰菊酯添加水平在7~20 μg/kg时, 回收率在95.9%~113.6%之间, 相对标准差在4.1%~10.8%之间, 定量限为7 μg/kg。结论 该方法具有简单、高效、准确等特点, 可用于海参中扑草净和甲氰菊酯残留量的定性与定量测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of prometryn and fenpropathrin residue in Apostichopus japonicus by solid-phase extraction-gas chromatography-mass spectrometry (SPE-GC/MS). Methods The samples were extracted with acetonitrile. The extracts were purified using a Cleanert Florisil solid-phase extraction column and then reconstituted in n-hexane. Matrix-matched standard solutions were prepared, and detection was performed in selected ion monitoring mode. The effects of different extraction solvents, solvent volumes, solid-phase extraction columns and elution ratios on extraction efficiency were compared. Results At spiked levels of 5–20 μg/kg, the recoveries of prometryn ranged from 86.3% to 106.0%, with relative standard deviations of 5.4%–11.6%, and the limit of quantitation was 5 μg/kg. For fenpropathrin at spiked levels of 7–20 μg/kg, the recoveries ranged from 95.9%–113.6%, with relative standard deviations of 4.1%–10.8%, and the limit of quantitation was 7 μg/kg. Conclusion This method is simple, efficient and accurate, making it suitable for both qualitative and quantitative determination of prometryn and fenpropathrin residues in Apostichopus japonicus.