高效液相色谱-串联质谱法研究猪组织中磺胺间甲氧嘧啶和磺胺二甲嘧啶的消除规律

Study on elimination regularity of sulfamonomethoxine and sulfadimidine in pig tissues by high performance liquid chromatography- tandem mass spectrometry

中文关键词:  磺胺间甲氧嘧啶  磺胺二甲嘧啶  猪组织  高效液相色谱-串联质谱法  消除规律

英文关键词:sulfamonomethoxine  sulfadimidine  pig tissues  high performance liquid chromatography-tandem mass spectrometry  elimination regularity

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)检测猪组织中磺胺间甲氧嘧啶(sulfamonomethoxine, SMM)和磺胺二甲嘧啶(sulfadimidine, SM2)残留的方法, 并初步进行磺胺间甲氧嘧啶和磺胺二甲嘧啶在猪组织中的消除规律研究。 方法 通过饲喂实验获得样品, 样品用乙腈提取, 浓缩定容后, 正己烷除脂, 高效液相色谱-串联质谱法检测, 外标法定量。结果 磺胺间甲氧嘧啶和磺胺二甲嘧啶在1~200 ng/mL浓度时, 线性良好, 相关系数r≥0.999, 检出限0.5 μg/kg、定量限1.0 μg/kg, 在1、10、200 μg/kg浓度添加时, 平均回收率为80.4%~92.4%; 2种药物在猪肉和猪肝中残留量没有显著差异, 停药28 d后未能检出药物。结论 该方法简便、快速、灵敏, 能够大批量操作, 磺胺间甲氧嘧啶和磺胺二甲嘧啶同时使用会造成磺胺间甲氧嘧啶利用率降低, 停药28 d后这2种药物均能完全代谢消除。

英文摘要:

      Objective To establish a method for the determination of sulfamonomethoxine and sulfadimidine residues in pig tissues by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), and study the elimination rule of sulfamonomethoxine and sulfadimidine in pig tissues. Methods The samples obtained from the feeding experiment were extracted with acetonitrile, concentrated to volume, degreased with n-hexane, detected by HPLC-MS/MS and quantified by external standard method. Results The linearities were good for sulfamonomethoxine and sulfadimidine at concentrations of 1-200 ng/mL, with correlation coefficients r≥0.999, and limits of detection were 0.5 μg/kg and limits of quantitation were 1.0 μg/kg. When the concentrations of 1, 10 and 200 μg/kg were added, the average recoveries were 80.4%?92.4%. There was no significant difference in the residues of the 2 drugs in pork and liver, and no drugs could be detected after 28 d of drug discontinuation. Conclusion This method is simple, rapid, sensitive and can be operated in large quantities. The simultaneous use of sulfamonomethoxine and sulfadimidine will reduce the utilization rate of sulfamonomethoxine, and these two drugs can be completely eliminated by metabolism after 28 days of drug withdrawal.