高效液相色谱-串联质谱法同时测定猪肉和牛肉中地塞米松、倍他米松、氟苯尼考及氟苯尼考胺残留量

Simultaneous determination of dexamethasone, betamethasone, florfenicol and florfenicol amine residues in pork and beef by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  地塞米松  倍他米松  氟苯尼考  氟苯尼考胺  高效液相色谱串联质谱法  猪肉  牛肉

英文关键词:dexamethasone  betamethasone  florfenicol  florfenicol amine  high performance liquid chromatography-tandem mass spectrometry  pork  beef

中文摘要:

      目的 建立高效液相色谱-串联质谱法同时测定猪肉和牛肉中地塞米松、倍他米松、氟苯尼考及氟苯尼考胺残留量的方法。方法 样品采用乙腈提取, 通过QuEChERS净化方式, 使用BEH-C18柱分离, 以乙腈和一级水作为流动相进行梯度洗脱, 在正负离子同时扫描下采用多反应监测, 进行外标法的定性定量分析。结果 地塞米松、倍他米松、氟苯尼考和氟苯尼考胺在0.2~100.0 ng/mL质量浓度下线性关系良好, 相关系数大于0.9990, 回收率在85.1%~107.5%之间。地塞米松的检出限(limits of detection, LODs)为0.44~0.48 μg/kg, 定量限(limits of quantitation, LOQs)为1.45~1.58 μg/kg; 倍他米松的LODs为0.46~0.51 μg/kg, LOQs为1.52~1.68 μg/kg; 氟苯尼考的LODs为0.47~0.58 μg/kg, LOQs为1.55~1.91 μg/kg; 氟苯尼考胺的LODs为0.40~0.45 μg/kg, LOQs为1.32~1.49 μg/kg。结论 该方法对参数测定准确, 具有较好的回收率和精密度, 同时前处理操作简单便捷, 满足日常猪肉和牛肉中地塞米松、倍他米松、氟苯尼考及氟苯尼考胺的同时筛查和定性定量检测, 可为日常风险评估提供参考价值。

英文摘要:

      Objective To establish a method for the simultaneous determination of dexamethasone, betamethasone, florfenicol and florfenicol amine residues in pork and beef by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile and purified using the QuEChERS method. Separation was performed on a BEH-C18 column with acetonitrile and ultrapure water as the mobile phase for gradient elution. Qualitative and quantitative analysis was conducted via multiple reaction monitoring under both positive and negative ion scanning modes using the external standard method. Results Dexamethasone, betamethasone, florfenicol and florfenicol amine exhibited excellent linearity within the mass concentration range of 0.2–100.0 ng/mL, with correlation coefficients exceeding 0.9990. The recovery rates ranged from 85.1% to 107.5%. The limits of detection (LODs) for dexamethasone were 0.44–0.48 μg/kg and the limits of quantitation (LOQs) were 1.45–1.58 μg/kg. For betamethasone, the LODs were 0.46–0.51 μg/kg and the LOQs were 1.52–1.68 μg/kg. For florfenicol, the LODs were 0.47–0.58 μg/kg and LOQs were 1.55–1.91 μg/kg. For florfenicol amine, the LODs were 0.40–0.45 μg/kg and the LOQs were 1.32–1.49 μg/kg. Conclusion This method demonstrates accurate parameter determination, with excellent recovery rates, high precision, and a simple, convenient pretreatment process. It meets the requirements for simultaneous screening and qualitative and quantitative detection of dexamethasone, betamethasone, florfenicol and florfenicol amine residues in pork and beef, thereby providing a reliable tool for routine risk assessment.