超高效液相色谱-串联质谱法测定干辣椒中2种新型杀虫剂残留量
目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定干辣椒中氰氟虫腙和氯虫苯甲酰胺残留量的分析方法。方法 干辣椒样品经乙腈匀浆提取, 氨基固相萃取小柱净化, 甲醇/水(50:50, V:V)定容, 以反相C18色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 0.1%甲酸-水和甲醇作为流动相进行梯度洗脱, 多反应监测模式下进行超高效液相色谱-串联质谱测定、基质匹配标准溶液外标法定量。结果 2种新型杀虫剂在5~500 μg /L范围内线性关系良好, 相关系数均大于0.999, 定量限为0.008~0.01 mg /kg; 在高、中、低3个加标水平下的回收率为80.4%~94.9%, 相对标准偏差在0.9%~8.7%之间。结论 方法简单、快速、灵敏高、准确可靠, 可操作性强, 适合测定干辣椒中氰氟虫腙和氯虫苯甲酰胺残留量。
Objective To establish a method for determination of metaflumizone and chlorantraniliprole in dried chilli by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with acetonitrile, and purified by amino solid phase extraction column, then methanol and water (50:50, V:V) were used for constant volume. They were separated on reverse C18 column with methanol and 0.1% formic acid (V:V) as the mobile phases in gradient program. The analytes were determined by UPLC-MS/MS under multiple reaction monitoring mode, and quantified by matrix matched external standard method. Results Good linearities were obtained for two new insecticides in the concentration range of 5~500 μg/L with correlation coefficients more than 0.999, and the limits of quantification were 0.008-0.01 mg/kg. The recoveries of the two insecticides were 80.4%-94.9% and the relative standard deviations were 0.9%-8.7% spiked at low, intermediate and high concentration levels. Conclusion The method is simple, sensitive and accurate, which is suitable for determination of two new insecticides in dried chilli.
标题：超高效液相色谱-串联质谱法测定干辣椒中2种新型杀虫剂残留量
英文标题：Determination of residual amounts of 2 kinds of new insecticides in dried chilli by ultra performance liquid chromatography-tandem mass spectrometry
作者：
刘炜 四川省农业科学院分析测试中心
刘行 四川省农业科学院经济作物育种栽培研究所
杨晓凤 四川省农业科学院分析测试中心
魏超 四川省农业科学院分析测试中心
尹全 四川省农业科学院分析测试中心
张义蓉 四川省农业科学院分析测试中心
罗晓梅 四川省农业科学院分析测试中心
中文关键词:干辣椒,氰氟虫腙,氯虫苯甲酰胺,超高效液相色谱-串联质谱法,
英文关键词:dried chilli,metaflumizone,chlorantraniliprole,ultra performance liquid chromatography-tandem mass spectrometry,
发表日期：2018-07-11
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