QuEChERS-超高效液相色谱-质谱法同时测定豆芽中9种氟喹诺酮类药物和植物生长调节剂

Simultaneous determination of 9 kinds of fluoroquinolones and plant growth regulators in bean sprouts by QuEChERS-ultra performance liquid chromatography-mass spectrometry

中文关键词:  豆芽、喹诺酮、生长调节剂、QuEChERS、超高效液相色谱-质谱联用法

英文关键词:bean sprouts  fluoroquinolones  growth regulators  QuEChERS  high performance liquid chromatography- mass spectrometry.

中文摘要:

      目的 建立一种QuEChERS-超高效液相色谱-质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)能够快速、稳定地同时测定豆芽中多种氟喹诺酮类以及生长调节剂药物残留的分析方法。方法 样品粉碎, 经甲酸乙腈提取, 净化包材料净化后, 通过保留时间匹配以及母离子、主要碎片离子的精确质量数进行定性分析、基质标准溶液外标定量的方法进行分析。结果 在优化条件下, 9种药物保留时间在4.9~8.8 min。质量浓度范围在0.010~0.200 μg/mL时, 9种参数的线性关系良好, 其相关系数为0.9149~0.9599, 检出限为5~10 μg/kg, 定量限为10~20 μg/kg, 空白样品的加标回收率为64.8%~135.5%, 相对标准偏差为1.05%~12.91%。结论 该方法操作简单、准确, 可快速定性定量分析豆芽中9种氟喹诺酮类药物和植物生长调节剂的残留, 对实现豆芽种植过程管控、日常监管、质量保障具有重要意义。

英文摘要:

      Objective To establish a QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry method for rapid and stable determination of residues of fluoroquinolones and growth regulators in bean sprouts. Methods The samples were crushed, extracted with acetonitrile-formic acid, purified using cleanup materials, and then analyzed through qualitative analysis based on retention time matching, precise mass numbers of parent ions and major fragment ions, as well as quantitative analysis using external standard calibration with matrix standard solutions. Results Under optimized conditions, the retention times of 9 kinds of drugs ranged from 4.9–8.8 minutes. Good linear relationships between the 9 kinds of parameters and quality concentration levels ranging from 0.010–0.200 μg/mL were observed, with correlation coefficients ranging from 0.9149–0.9599. The limits of detection ranged from 5–10 μg/kg, while quantification limits ranged from 10–20 μg/kg. The recovery rates of blank samples spiked with standards were between 64.8% and 135.5%, with relative standard deviations ranging from 1.05%–12.91%. Conclusion This method is simple and accurate, and can be used for rapid qualitative and quantitative analysis of residual fluoroquinolone drugs and plant growth regulatorsin bean sprouts. It holds significant importance for implementing process control, daily supervision, and quality assurancein bean sprout cultivation processes.