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超高效液相色谱法测定西瓜中的喹啉铜残留量

Determination of Copper 8-Quinolinolate Residues in Watermelon by Ultra Performance Liquid Chromatography

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【作者】 李雨晨李腾邓立刚李增梅刘俊华岳晖赵善仓

【Author】 LI Yu-chen;LI Teng;DENG Li-gang;LI Zeng-mei;LIU Jun-hua;YUE Hui;ZHAO Shan-cang;Academy of Food Science and Engineering,Shandong Agricultural University;Institute of Agricultural Quality Standards and Testing Technology Research,Shandong Academy of Agricultural Sciences;Key Laboratory of Test Technology on Food Quality and Safety of Shandong Province;

【机构】 山东农业大学食品科学与工程学院山东农业科学院农业质量标准与检测技术研究所山东省食品质量与安全检测技术重点实验室

【摘要】 建立了西瓜样品中喹啉铜农药残留的超高效液相色谱分析方法。样品用4%冰醋酸超声振荡提取,提取液经阳离子交换固相萃取小柱净化后,用1%醋酸铵-甲醇洗脱,洗脱液经氮气吹干后用流动相定容。试样采用Vneusil MP C18色谱柱(150 mm×4.6 mm,5μm)进行分离,流动相为0.1%三氟乙酸-乙腈(95∶5)。结果表明,喹啉铜在0.05~10μg/mL浓度范围内线性关系良好,相关系数不低于0.999 9。在0.05~2.0 mg/kg加标浓度范围内的平均回收率为72.3%~84.1%,相对标准偏差为2.1%~3.8%,方法的检出限为0.024 mg/kg。

【Abstract】 A novel method for the determination of copper 8-quinolinolate by ultra-performance liquid chromatography(UPLC) was developed.The sample was extracted with 4% acetic acid solution and cleaned up with a Cleanert PCX cartridge.The cartridge was eluted with 1% ammonium acetate-methanol.The elution was evaporated to near dryness under a stream of nitrogen,and dissolved by mobile phase.The target compound was separated on a Vneusil MP C18column(150 mm × 4.6 mm,5 μm) using 0.1% TFA-acetonitrile(95 ∶ 5) as mobile phase.The method had a good linear correlation(r≥0.999 9)in the range of 0.05-10 μg/mL.The average recoveries of copper 8-quinolinolate at a spiked range of 0.05-2.0 mg/kg were in the range of 72.3%-84.1% with relative standard deviations(RSDs)of 2.1%-3.8%.The limit of detection(LOD) was 0.024 mg/kg.

【基金】 山东省重点实验室开放课题资助(2013KF04)
  • 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2014年08期
  • 【分类号】O657.72;TS255.7
  • 【被引频次】14
  • 【下载频次】252
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