超高效液相色谱-串联质谱法同时测定药食同源食品中9种双酰胺类杀虫剂残留量

Simultaneous determination of 9 kinds of diamide insecticides residues in medicinal and edible homologous food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱  药食同源  双酰胺  杀虫剂

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  medicinal and edible homologous food  diamide  insecticides

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)测定药食同源食品中9种双酰胺类杀虫剂农药残留的分析方法。方法 本研究选择枸杞、桑葚、菊花、当归4种药食同源食品样品称样量为2.00 g, 提取试剂为0.1%甲酸酸化乙腈, 提取方式为涡旋振荡5 min结合超声10 min, 萃取盐为4 g无水硫酸镁+1 g氯化钠+1 g柠檬酸钠二水合物+0.5 g柠檬酸二钠盐倍半水合物, 净化方式为每毫升提取液使用150 mg无水硫酸镁、50 mg C18和50 mg N-丙基乙二胺(primary secondary amine, PSA)。结果 在2.0~100.0 μg/L范围内, 9种双酰胺类杀虫剂线性相关系数大于0.999, 本研究方法具有良好的稳定性和重复性。检出限为3.0 μg/kg, 定量限为10.0 μg/kg。当样品加标水平为10、20和100 μg/kg时, 回收率为70.6%~96.0%, 相对标准偏差为3.4%~9.0% (n=6)。结论 本研究针对现有双酰胺类杀虫剂残留检测方法的不足, 建立了更加全面有效的检测方法, 提高了药食同源食品中农药残留的检测质量, 对保障药食同源食品的食用安全具有重要的应用价值。

英文摘要:

      Objective To establish a analytical method for detecting pesticide residues of 9 kinds of diamide insecticides in medicinal and edible homologous food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods In this experiment, 2.00 g of 4 kinds of medicinal and edible homologous food samples: Lycium barbarum, Fructus Mori, Chrysanthemum morifolium Ramat and Angelica sinensis were selected. The extraction solvent was 0.1% formic acid in acetonitrile, and the extraction procedure involved vortex oscillation for 5 min followed by ultrasonication for 10 min. The extraction salts used were 4 g magnesium sulfate+1 g NaCl+1 g C6H5Na3O7·2H2O+0.5 g C6H6Na2O7·1.5 H2O. The purification method employed 150 mg MgSO4, 50 mg C18 and 50 mg primary secondary amine (PSA) per milliliter of extract. Results The results showed that within the range of 2.0–100.0 μg/L, the linear correlation coefficient of 9 kinds of diamide insecticides was greater than 0.999, the method developed in this study demonstrates excellent stability and repeatability. Limit of detection was 3.0 μg/kg and the limit of quantitation was 10.0 μg/kg. When the sample was spiked at levels of 10, 20 and 100 μg/kg, the recovery rates were 70.6%-96.0% and relative standard deviations were 3.4%-9.0% (n=6). Conclusion This study addresses the limitations of existing detection methods for diamide insecticide residues by developing a more comprehensive and effective analytical method. The improved methodology enhances the accuracy and reliability of pesticide residue detection in medicinal and edible homologous food, demonstrating significant practical value in ensuring the food safety of these dual-purpose items.