刘炜,刘行,杨晓凤,魏超,尹全,张义蓉,罗晓梅.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[J].食品安全质量检测学报,2018,9(18):4971-4974
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
Determination of residual amounts of 2 kinds of new insecticides in dried chilli by ultra performance liquid chromatography-tandem mass spectrometry
投稿时间:2018-07-11  修订日期:2018-08-20
DOI:
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
基金项目:
作者单位
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 
AuthorInstitution
LIU Wei Analysis and Testing Center of Sichuan Academy of Agricultural Sciences 
LIU Xing Economic Crops Research Institute, Sichuan Academy of Agricultural Sciences 
YANG Xiao-Feng Analysis and Testing Center of Sichuan Academy of Agricultural Sciences 
WEI Chao Analysis and Testing Center of Sichuan Academy of Agricultural Sciences 
YIN Quan Analysis and Testing Center of Sichuan Academy of Agricultural Sciences 
ZHANG Yi-Rong Analysis and Testing Center of Sichuan Academy of Agricultural Sciences 
LUO Xiao-Mei Analysis and Testing Center of Sichuan Academy of Agricultural Sciences 
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中文摘要:
      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。
英文摘要:
      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.
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