优化的QuEChERS-超高效液相色谱-串联质谱法测定韭菜中31种农药残留 |
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引用本文: | 李浩林,李桐桐,董玉英,禾丽菲,李北兴,慕卫.优化的QuEChERS-超高效液相色谱-串联质谱法测定韭菜中31种农药残留[J].农药学学报,2021,23(3):603-606. |
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作者姓名: | 李浩林 李桐桐 董玉英 禾丽菲 李北兴 慕卫 |
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作者单位: | 1.山东农业大学 植物保护学院 农药毒理与应用技术重点实验室,山东 泰安 271018 |
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基金项目: | 国家自然科学基金 (32072463;32001953) |
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摘 要: | 基于超高效液相色谱-串联质谱 (UPLC-MS/MS),建立了同时检测韭菜中31种农药残留的分析方法。韭菜样品经乙腈提取,采用优化的QuEChERS方法净化后,进行UPLC-MS/MS 检测。结果表明:在 0.5~100 μg/L范围内,31种农药的质量浓度与相应峰面积间呈良好的线性关系,相关系数均大于0.995,定量限 (LOQs) 为0.01 mg/kg;在0.01、0.1和1 mg/kg 3个添加水平下,31种农药在韭菜中的平均回收率在70%~102%之间,相对标准偏差 (RSD) 均小于11% (n = 5)。该方法快速、简便、可靠、高效,且成本低廉,适用于同时检测韭菜中多种农药的残留量。
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关 键 词: | QuEChERS 超高效液相色谱-串联质谱 韭菜 农药 多残留分析 |
收稿时间: | 2020-10-02 |
Determination of 31 pesticide residues in Chinese chives by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry |
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Institution: | 1.Key Laboratory of Pesticide Toxicology and Application Technology, College of Plant Protection, Shandong Agricultural University, Tai’an 271018, Shandong Province, China2.Baiyunshan School in Feicheng, Tai’an 271699, Shandong Province, China |
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Abstract: | Based on QuEChERS and ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), a method for simultaneous detection of 31 pesticide residues in Chinese chives was established. The Chinese chive samples were extracted by acetonitrile, cleaned-up by modified QuEChERS method and then analyzed by UPLC-MS/MS. Results showed that good linear relationship was obtained between the mass concentrations of 31 pesticides and the corresponding peak areas in the range of 0.5-100 μg/L with all of the correlation coefficients higher than 0.995, and the LOQs (limits of quantification) of the pesticides were all 0.01 mg/kg. The average recoveries of 31 pesticides ranged from 70%-102% at the spiking level of 0.01, 0.1 and 1 mg/kg with RSDs lower than 11% (n = 5). The method was rapid, simple, reliable, efficient, and low cost, and was suitable for simultaneous determination of 31 pesticide multi-residues in Chinese chives. |
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