超高效液相色谱-串联质谱法检测柑橘中的氟唑菌酰胺残留量

Determination of fluxapyroxad residues in citrus by ultra performance liquid chromatography- tandem mass spectrometry

中文关键词:  氟唑菌酰胺  超高效液相色谱-串联质谱法  柑橘  残留  消解

英文关键词:fluxapyroxad  ultra performance liquid chromatography-tandem mass spectrometry  citrus  residue  digestion

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)测定柑橘中氟唑菌酰胺的分析方法。方法 样品采用乙腈提取, 选取Acquity UPLC BEH C18 (2.1 mm×100 mm, 1.7 μm)色谱柱对氟唑菌酰胺进行分离, 以0.1%甲酸-乙腈作为流动相进行梯度洗脱, 使用电喷雾正离子电离模式进行数据收集, 采用基质匹配外标法对氟唑菌酰胺进行定量分析。结果 使用量为50 mg乙二胺-N-丙基硅烷化硅胶(ethylenediamine-N-propylsilane, PSA)和300 mg无水硫酸镁时净化效果最佳。氟唑菌酰胺在柑橘全果中的加标回收率为89.1%~105.5%, 相对标准偏差(relative standard deviation, RSD)≤1.18%。氟唑菌酰胺在果肉中的加标回收率为93.4%~104.4%, RSD≤1.41%。氟唑菌酰胺在全果和果肉中的消解半衰期分别为13.56 d和10.56 d。在采样时间分别为距离最后1次施药后第14 d和第21 d时, 氟唑菌酰胺在柑橘全果中的残留量为0.206、0.178 mg/kg; 在柑橘果肉中的残留量为0.028、0.020 mg/kg。结论 该方法灵敏度较高、操作简单, 准确度与精密度均能达到定量分析要求, 适用于柑橘中氟唑菌酰胺的检测; 根据氟唑菌酰胺在柑橘中的残留实验结果, 推荐施药剂量为不超过稀释2500倍液的制剂用量, 且最多施药3次, 安全间隔期(10 d)以21 d为宜。

英文摘要:

      Objective To establish a method for the determination of fluxapyroxad in citrus by ultra performance liquid chromatography-quadrupole tandem mass spectrometry (UPLC-MS/MS). Methods The sample was extracted with acetonitrile, and the separation was processed in a C18 (2.1 mm×100 mm, 1.7 μm) column. The gradient elution was carried out with 0.1% formic acid and acetonitrile as mobile phase, and electrospray positive ion scanning and multi-response monitoring pattern detection were used. The matrix matching external standard method was utilized for quantification. Results The best purification effect was obtained when 50 mg PSA and 300 mg magnesium sulfate (anhydrous) were selected for purification. The recoveries of fluxapyroxad in citrus fruit were 89.1%?105.5%, and the relative standard deviation (RSD) was less than or equal to 1.18%. And in citrus pulp, the recoveries were 93.4%?104.4%, and the RSD was less than or equal to 1.41%. When the sampling time was 14 days and 21 days after the last application, respectively, the residue of fluxapyroxad in whole citrus fruit were 0.206, 0.178 mg/kg, the digestion half-life was 13.56 days, and the residue in citrus pulp were 0.028, 0.020 mg/kg, and the digestion half-life was 10.56 days. Conclusion The method is sensitive, simple and convenient, and the accuracy and precision can meet the requirements of quantitative analysis of fluxapyroxad. It is suitable for the determination of fluxapyroxad in citrus. According to the results of residue test of fluxapyroxad in citrus, the recommended dosage is not more than 2500 times of dilution, and the maximum dosage is 3 times. The safe interval (10 days) is 21 days.