Sin-QuEChERS结合超高效液相色谱串联质谱法同时检测果蔬中5种双酰胺类杀虫剂

Simultaneous determination of 5 kinds of diamide insecticides in fruits and vegetables by Sin-QuEChERS with ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  Sin-QuEChERS  超高效液相色谱串联质谱法  溴氰虫酰胺  氯虫苯甲酰胺  四氯虫酰胺  环溴虫酰胺  氟苯虫酰胺  双酰胺类杀虫剂

英文关键词:Sin-QuEChERS  ultra performance liquid chromatography tandem mass spectrometry  cyantraniliprole  chlorantraniliprole  tetrachlorantraniliprole  cyclaniliprole  flubendiamide  diamide insecticide

中文摘要:

      目的 建立Sin-QuEChERS结合超高效液相色谱串联质谱法同时检测水果和蔬菜中溴氰虫酰胺、氯虫苯甲酰胺、四氯虫酰胺、环溴虫酰胺、氟苯虫酰胺5种新型双酰胺类杀虫剂的分析方法。方法 样品经乙腈提取后, 经新颖的基质分散净化装置(Sin-QuEChERS)净化, 采用C18色谱柱进行分离, 以水和乙腈为流动相进行梯度洗脱, 质谱采用电喷雾电离, 多反应监测模式, 其中溴氰虫酰胺、氯虫苯甲酰胺采用正离子模式, 四氯虫酰胺、环溴虫酰胺、氟苯虫酰胺采用负离子模式。结果 5种化合物在1~100 μg/L浓度范围内线性关系良好, 相关系数(r2)为0.9987~0.9999。在5、10、50 μg/kg 3个添加水平下的平均回收率为73.0%~115.8%, 相对标准偏差小于10.9%(n=6), 方法定量限为5 μg/kg。结论 该方法快速简便、检测准确、灵敏度高, 适合水果蔬菜中溴氰虫酰胺、氯虫苯甲酰胺、四氯虫酰胺、环溴虫酰胺、氟苯虫酰胺的残留检测。

英文摘要:

      Objective To establish a method for simultaneous determination of 5 new diamide insecticides including cyantraniliprole, chlorantraniliprole, tetrachlorantraniliprole, cyclaniliprole, flubendiamide in fruits and vegetables by Sin-QuEChERS with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by acetonitrile, purified by a novel pressing of the Sin-QuEChERS packing column, separated by C18 column with water and acetonitrile as mobile phases for gradient elute, then analyzed by UPLC-MS/MS. The mass spectrometry was operated in electronic spay ionization (ESI) mode with dynamic multiple reaction monitoring (MRM), cyantraniliprole, chlorantraniliprole were analyzed with positive ion mode while tetrachlorantraniliprole, cyclaniliprole, flubendiamide were analyzed with negative ion mode. Results The calibration curves of the 5 compounds showed an excellent linearity in the range of 1-100 μg/L, the correlation coefficient (r2) were between 0.9987 and 0.9999. The average recoveries were in the range of 73.0%-115.8% with three spiked levels of 5, 10 and 50 μg/kg. The relative standard deviations (RSDs) were less than 10.9% (n=6), and the limits of quantitation (LOQs) for the five compounds were 5 μg/kg. Conclusion The proposed method is efficient, reliable and sensitive, which can be used for the determination of cyantraniliprole, chlorantraniliprole, tetrachlorantraniliprole, cyclaniliprole, flubendiamide in fruits and vegetables.