| 郑龙，杨春亮，曾少东.超高效液相色谱串联质谱测定化橘红中阿维菌素等4 种农药残留的分析方法[J].广东农业科学,2014,41(23):102-105 |
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超高效液相色谱串联质谱测定化橘红中阿维菌素等4 种农药残留的分析方法 |
| Determination of abamectin and other three pesticides in Citrus grandis‘Tomentosa’by HPLC-MS/MS |
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| DOI： |
| 中文关键词: HPLC-MS/MS 化橘红 农药残留 |
| 英文关键词: HPLC-MS/MS Citrus grandis‘Tomentosa’ pesticide residues |
| 基金项目:农产品质量安全风险评估应急处置财政专项（GJFP2014011） |
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| 中文摘要: |
| 建立化橘红中阿维菌素、吡虫啉、灭幼脲和噻嗪酮等4 种农药残留的液相色谱-串联质谱(HPLC-MS/MS)测定方法。试验样品用乙腈提取，经石墨化炭黑-氨基固相萃取小柱净化，以乙腈和5 mmol 乙酸铵水溶液为流动相梯度洗脱，采用多反应监测(MRM)模式检测。结果表明，4 种农药在5~200μg/L 范围内，线性关系良好，相关系数均在0.99 以上，检出限范围在0.1~0.5 μg/kg 之间。添加水平在10~200 μg/kg 范围时，加标回收率在81.9%~94.1%间，相对标准偏差在5.4%~9.2%之间。该方法操作简便快捷，结果准确可靠，能满足化橘红农药残留分析的要求。 |
| 英文摘要: |
| new method of determination and confirmation for four pesticide residues in Citrus grandis‘Tomentosa’was developed by HPLC-MS/MS. The sample was extracted with acetonitrile, and purified with a Carbon/NH2 SPE column, then washed with the gradient elution of acetonitrile and 5 mmol aqueous ammonium acetate. At last, the identification of target compounds were measured through MS under multiple reaction monitoring (MRM) mode. The results showed that when the amount of pesticide residues was in the range of 5-200 μg/L, it obtained good linear relation, and its relative coefficient was above 0.99. The detection limit was between 0.1-0.5 μg/kg. When the additional level was at 10-200 μg/kg, the recycle degree was in the range of 81.9%-94.1%, and the relative standard deviation was 5.4%-9.2%. This method
possessed simple operation and accurate result, which could meet the requirements for the determination of pesticides in C.grandis‘Tomentosa’. |
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