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苹果与土壤中虱螨脲残留的超高效液相色谱快速分析方法研究

Rapid Determination of Lufenuron Residue in Apple and Soil by Ultra Performance Liquid Chromatography

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【作者】 郭长英李增梅邬元娟梁京芸李腾张树秋

【Author】 GUO Chang-ying;LI Zeng-mei;WU Yuan-juan;LIANG Jing-yun;LI Teng;ZHANG Shu-qiu;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】 建立了简便、快速、灵敏的测定苹果和土壤中虱螨脲残留的超高效液相色谱分析方法。样品采用乙腈提取,提取液经盐析后无需净化,将上清液浓缩复溶,过膜后直接上机测试。试样采用BEH C18(50.0 mm×2.1 mm,1.7μm)色谱柱分离,甲醇-水(60∶40)为流动相等度洗脱后,紫外检测器检测,检测波长为255 nm。结果表明,虱螨脲在0.025~2.5 mg/L浓度范围内线性关系良好,相关系数为0.999 7。在0.05~0.5 mg/kg加标浓度范围内的平均回收率为84.5%~98.7%,相对标准偏差(RSD)为0.7%~6.1%,方法的检出限为0.01 mg/kg。

【Abstract】 A quantitative method using ultra performance liquid chromatography( UPLC) with UV detector was developed for the determination of lufenuron residue in apple and soil. The sample was extracted with acetonitrile and the extractants were separated from water caused by the addition of salts.The supernatant was concentrated to dryness without any further clean-up step,and the residue was redissolved with methanol and then diluted with water prior to HPLC analysis. A BEH C18column( 50. 0 mm × 2. 1 mm,1. 7 μm) was used to separate the sample by using a mixture of methanol-water( 60 ∶ 40) as mobile phase at a flow rate of 0. 4 m L / min. The ultraviolet detection wavelength was set at 255 nm. The method had a good linear relationship in the range of 0. 025- 2. 5 mg / L with a correlation coefficient( r) of 0. 999 7. The average recoveries of lufenuron at a spiked range of 0. 05- 0. 5 mg / kg ranged from 84. 5% to 98. 7% with relative standard deviations( RSDs) of 0. 7%-6. 1%. The limit of detection( LOD) was 0. 01 mg / kg.

【基金】 山东省自主创新及成果转化专项(201422CX02703);山东省农科院青年科研基金(2015YQN50);山东省科技专项基金(2011SJGZ18)
  • 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2015年10期
  • 【分类号】O657.72;S481.8
  • 【被引频次】4
  • 【下载频次】159
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