超高效液相色谱-串联质谱法同时测定水产品中4种酰胺醇类抗生素残留

Simultaneous determination of 4 kinds of amidol antibiotics residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  水产品  酰胺醇类  代谢物

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  aquatic products  amidol antibiotics  metabolite

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法同时测定水产品中酰胺醇类抗生素氯霉素、甲砜霉素、氟苯尼考及代谢物氟苯尼考胺残留的方法。方法 水产样品经乙腈提取, 正己烷除脂后, 在Capcell Pak ADME (100 mm×2.1 mm, 2.7 μm)色谱柱上分离, 采用多反应监测模式, 以氯霉素-D5和氟苯尼考胺-D3为内标进行定量测定。结果 氯霉素在0.5~25.0 ng/mL范围内线性关系良好(r>0.999), 甲砜霉素、氟苯尼考和氟苯尼考胺在5.0~250.0 ng/mL范围内线性关系良好(r>0.998)。方法检出限为0.1~1.0 μg/kg, 定量限为0.2~2.0 μg/kg。当氯霉素添加水平为0.2、1.0和10.0 μg/kg时, 回收率为82.5%~104.0%, 相对标准偏差在2.2%~11.8%之间; 当甲砜霉素、氟苯尼考和氟苯尼考胺添加水平为2.0、10.0和100.0 μg/kg时, 回收率为80.9%~102.0%, 相对标准偏差在0.8%~8.4%之间。结论 该方法快速简单、准确、成本低, 适用于水产品中4种酰胺醇类抗生素残留的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of chloramphenicol, thiamphenicol, florfenicol and florfenicol amine residues in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry. Methods The aquatic samples were extracted with acetonitrile, degreased with n-hexane, and separated on a Capcell Pak ADME (100 mm×2.1 mm, 2.7 m) chromatographic column, the multi-reaction monitoring mode was adopted for the quantitative determination with chloramphenicol-D5 and florfenicol amine-D3 as internal standards. Results The linear relationship of chloramphenicol was good in the range of 0.5?25.0 ng/mL (r>0.999), and that of thiamphenicol, florfenicol and florfenicol amine were good in the range of 5.0?250.0 ng/mL (r>0.998). The limits of detection were 0.1?1.0 μg/kg, and the limits of quantitative were 0.2?2.0 μg/kg, the recoveries were 82.5%?104.0% and the relative standard deviations were 2.2%–11.8% when chloramphenicol was added at 0.2, 1.0, and 10.0 μg/kg, respectively; when the addition levels of thiamphenicol, florfenicol, and florfenicol amine were 2.0, 10.0, and 100.0 μg/kg, the recoveries were 80.9%?102.0%, and the relative standard deviations were 0.8%?8.4%. Conclusion This method is rapid, simple, accurate and low in cost, and is suitable for the determination of the residues of 4 kinds of amidol antibiotics residues in aquatic products.