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›› 2015, Vol. 37 ›› Issue (3): 227-232.

• 论文与报告 • 上一篇    下一篇

气相色谱-质谱法测定甲壳类水产品中4-己基间苯二酚残留

余颖   

  1. 福建省水产研究所
  • 收稿日期:2015-03-03 修回日期:2015-04-16 出版日期:2015-06-25 发布日期:2015-06-23
  • 通讯作者: 余颖
  • 基金资助:
    福建省省属公益类科研院所基本科研专项;福建省海洋高新产业发展专项

Determination of 4-hexylresorcinol residue in crustacea by gas chromatography-mass spectrometry

  • Received:2015-03-03 Revised:2015-04-16 Online:2015-06-25 Published:2015-06-23

摘要: 研究建立了甲壳类水产品中4- 己基间苯二酚(4 - hexylresorcinol,4-HR) 残留量的固相萃取- 气相色谱- 质谱检测方法。样品采用乙酸乙酯提取,硅胶柱净化,乙酸乙酯洗脱,气相色谱- 质谱测定,外标法定量。4 - HR 的响应值与其质量浓度在0.05 ~ 10 μg/ mL范围内的线性关系良好,相关系数为0.9 997;0.05 ~ 1 mg/ kg 添加浓度的日内和日间平均回收率为76.8% ~102% ,相对标准偏差为2.43% ~7.65% ;检出限为0.01 mg/ kg,最低定量限为0.05 mg/ kg。该方法适用于甲壳类水产品中4- HR 残留的检测。

关键词: 4-己基间苯二酚, 气相色谱-质谱法, 甲壳类, 残留, 4-hexylresorcinol, gas chromatography-mass spectrometry, crustacean, residue

Abstract: Gas chromatography-mass spectrometry (GC-MS) coupled with solid-phase extraction was developed for determination of 4-hexylresorcinol residue in crustacean. The 4-HR was extracted with ethyl acetate, purified by silicagel column and eluted with ethyl acetate, the eluent was concentrated and dissolved in ethyl acetate-n-hexane(1:1,v/v), then analyzed by gas chromatography-mass spectrometry. The results showed that the linear range was 0.05 ~10 μg/mL and its correlation coefficient was 0.9 997.When spiked within 0.05~1 mg/kg, the average recoveries of intraday and intraday were 76.8%~102%, and their relative standard deviations were 2.43%~7.65%.The limits of detection and limits of quantitation were 0.01 mg/kg and 0.05 mg/kg, respectively. This method can be applied to determine the 4-HR residues in crustacea with the advantages of high extraction efficiency, high purification effect and less solvent consumption.

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