多壁碳纳米管净化-液相色谱串联质谱法测定瓜菜中双酰胺类杀虫剂
目的 建立多壁碳纳米管净化, 超高效液相色谱串联质谱技术同时测定瓜菜中3种双酰胺类杀虫剂残留的分析方法。方法 瓜菜样品用乙腈提取后, 经多壁碳纳米管净化, 超高效液相色谱-电喷雾电离串联质谱法测定。结果 3种双酰胺类杀虫剂在0.005~0.1 mg/L范围内线性良好, 相关系数均大于0.99, 定量限均为5 μg/kg, 平均加标回收率在71.7%~99.1%之间, 相对标准偏差在0.6%~3.5%之间。与N-丙基乙二胺和石墨化炭黑吸附剂相比, 多壁碳纳米管具有更好的净化性能。结论 该方法具有简单灵敏、定量准确等优点, 可用于瓜菜中3种双酰胺类杀虫剂残留的检测。
Objective To establish a multi-residue method for the simultaneous determination of 3 diamide insecticide residues in melons and vegetables by multiwalled carbon nanotubes purification coupled with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods The melon and vegetable samples were extracted with acetonitrile and cleaned up with multiwalled carbon nanotubes, then determined by UPLC-MS/MS. Results Three kinds of diamide insecticide had good linear relationships in the range of 0.005-0.1 mg/L, and the correlation coefficients were larger than 0.99. The limits of quantitation for 3 diamide insecticide were all 5 μg/kg. Calibration curves exhibited good linearity over the concentration range from 0.005 to 0.1 mg/L. Average recoveries for 3 diamide insecticide were 71.7%-99.1%, with relative standard deviations ranged of 0.6%-3.5%. Compared with primary secondary amine and graphited carbon black sorbent, the multiwalled carbon nanotube had better purification performance. Conclusion The developed method is simple, sensitive, and accurate, which can be used for determination of 3 diamide insecticide residues in melons and vegetables.
标题：多壁碳纳米管净化-液相色谱串联质谱法测定瓜菜中双酰胺类杀虫剂
英文标题：Determination of diamide insecticide residues in melons and vegetables using multiwalled carbon nanotubes purification coupled with ultra performance liquid chromatography tandem mass spectrometry
作者：
乐渊 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
刘春华 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
吴南村 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
赵敏 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室
杨衍 中国热带农业科学院热带作物品种资源研究所
中文关键词:瓜菜,双酰胺类杀虫剂,多壁碳纳米管,超高效液相色谱-串联质谱,
英文关键词:melons and vegetables,diamide insecticide,multiwalled carbon nanotube,ultra performance liquid chromatography tandem mass spectrometry,
发表日期：2019-03-27
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