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›› 2016, Vol. 38 ›› Issue (3): 244-253.

• 论文与报告 • 上一篇    下一篇

利用不确定度评定对改进后水产品中喹乙醇的检测方法进行确证研究

张惠峰,闫先春,甄昕   

  1. 长春市水产品质量安全检测中心
  • 收稿日期:2016-05-27 修回日期:2016-06-03 出版日期:2016-06-27 发布日期:2016-07-18
  • 通讯作者: 张惠峰
  • 基金资助:
    长春市水产品质量安全风险评估专项

Evaluation of uncertainty was used to verify a new improved detection method on Olaquindox in aquatic products

  • Received:2016-05-27 Revised:2016-06-03 Online:2016-06-27 Published:2016-07-18
  • Contact: Hui-Feng ZHANG

摘要: 建立了水产品中喹乙醇测定的改进方法。改进了前处理方式,样品用热水提取后,经硅藻土和正己烷净化,并对色谱条件进行优化,从而提高检测效率。结果表明,改进后的方法高效简易、灵敏准确,在4个不同基质样品的2个加标水平下的平均回收率为77.2%~87.0%,相对标准偏差为0.4%~6.3%,检出限10 μg/kg,定量限30 μg/kg 。建立了不确定度评定数学模型,通过计算和分析测量过程中各不确定度,对方法和测试条件进行确证。测量系统相对不确定度小于8%,主要受测量过程的随机效应、标准曲线拟合、回收率等因素影响。该方法高效便捷、准确可靠、快速且节约成本,适用于水产品中喹乙醇的检测。此外,本研究对利用不确定度评定进行检测方法确证有十分重要的指导意义。

关键词: 喹乙醇, 不确定度, 水产品, 检测, 确证, Olaquindox, uncertainty, aquatic product, detection, verify

Abstract: An improved method was established for the detection of Olaquindox in aquatic products. An improved pre-treatment method was used in this study. The samples were extracted with hot water and separated by diatomite and n-Hexane,and the chromatographic parameters were optimized, so detection efficiency was raised significantly. The results showed that the average recoveries at two different samples and four different spiked levels was 77.2%~87.0%, the relative standard deviation of 0.4%~6.3%, the detection limit 10 μg/kg, the limit of quantification 30 μg/kg. A mathematical model of uncertainty evaluation was established. Reliability and test conditions were verified by uncertainty analysis and calculation. Relative uncertainty of this method was less than 8%, which was affected by random effect and calibration curve and recovery. This method is not only simple and sensitive and accurate, but also rapid and cost savings,so it is very suitable for the determination of Olaquindox in aquatic products. This study that uncertainty evaluation is used to verify the detection method is very important.