Captiva EMR-Lipid固相萃取结合高效液相色谱-串联质谱法同时测定猪肉中氯霉素类药物残留量

Simultaneous determination of chloramphenicol drugs residues in pork by Captiva EMR-Lipid solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  Captiva EMR-Lipid固相萃取  高效液相色谱-串联质谱法  氯霉素  甲砜霉素  氟苯尼考  猪肉

英文关键词:Captiva EMR-Lipid solid phase extraction  high performance liquid chromatography-tandem mass spectrometry  chloramphenicol  thiamphenicol  florfenicol  pork

中文摘要:

      目的 建立Captiva EMR-Lipid固相萃取结合高效液相色谱-串联质谱法同时测定猪肉中氯霉素、甲砜霉素和氟苯尼考残留量的分析方法。方法 采用乙腈提取样品, 经Captiva EMR-Lipid固相萃取柱净化, 以甲醇-水为流动相, CNW Athena C18-WP色谱柱(100 mm×2.1 mm, 3 μm)进行分离, 采用电喷雾负离子扫描和多反应监测模式, 内标法定量。结果 氯霉素、甲砜霉素和氟苯尼考在0.5~20.0 ng/mL范围内呈现良好的线性关系(r＞0.9975), 方法的检出限为0.10~0.14 ?g/kg, 定量限为0.25~0.47 ?g/kg, 平均回收率为97.50%~117.00%, 相对标准偏差为5.55%~8.93%。结论 该方法简单快速、稳定可靠, 适用于猪肉中氯霉素、甲砜霉素和氟苯尼考的同时测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of chloramphenicol, thiamphenicol and florfenicol residues in pork by Captiva EMR-Lipid solid phase extraction-high performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with acetonitrile, purified by Captiva EMR-Lipid solid phase extraction column, separated by CNW Athena C18-WP chromatographic column (100 mm× 2.1 mm, 3 μm) with methanol-water as mobile phase, the analyte was determined by electrospray negative ion scanning mode and multiple reaction monitoring mode with internal standard method for quantification. Results The method had good linear relationship in the range of 0.5?20.0 ng/mL for chloramphenicol, thiamphenicol and florfenicol (r＞0.9975), the limits of detection were 0.10?0.14 ?g/kg, the limits of quantification were 0.25?0.47 ?g/kg, the average recoveries were 97.50%?117.00%, and the relative standard deviations were 5.55%?8.93%. Conclusion This method is simple and fast, stable and reliable, and suitable for the simultaneous determination of chloramphenicol, thiamphenicol and florfenicol in pork.