超高效液相色谱-串联质谱法测定猪组织中泰拉霉素及其代谢物残留量

Determination of Tulathromycin and its Metabolites in pig tissue by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

关键词:  超高效液相色谱-串联质谱法  泰拉霉素  猪组织

Key words:  ultra-high performance liquid chromatography-tandem mass spectrometry  tulathromycin  pig tissues

摘要:

通过对猪组织中泰拉霉素及其代谢物残留量的测定方法研究，基于超高效液相色谱-串联质谱建立了猪肉、肝脏、肾脏中泰拉霉素及其代谢物残留量的测定方法。试样经乙腈-0.1%甲酸水（7+3）提取，MCX柱净化，氮吹后用乙腈-0.1%甲酸水（1+9）复溶，正离子扫描，多反应监测模式下上机分析，基质外标法定量。结果表明，泰拉霉素及其代谢物在5~500 μg/kg的浓度范围内呈现良好的线性关系，相关系数（R2）均＞0.99；该方法的检出限为5 μg/kg（猪肉：2 μg/kg），定量限为10 μg/kg；在不同浓度添加水平下，平均回收率为72.6%-105.8%，日内相对标准偏差为0.5%-12.1%，日间相对标准偏差为2.9%-8.1%。该方法简便、快速、灵敏度高、重现性好，适用于猪组织中泰拉霉素及其代谢物残留量的测定。

Abstract:

A method for the determination of tulathromycin and its metabolites in pig tissue was developed by ultra-high performance liquid chromatography-tandem mass spectrometry . The samples were extracted by acetonitrile-0.1% formic acid aqueous (7+3) and cleaned by MCX solid phase extraction column, and the residue was redissolved with acetonitrile-0.1% formic acid aqueous (1+9) after the dried under a N2 atmosphere. In the positive ion mode and multi reaction monitoring mode, the analytes were quantified by matrix external standard. The results of tulathromycin and its metabolites were linear in the range of 5~500 μg/kg with the correlation coefficients (R2) ＞0.99. The limits of detection (LODs) and the limits of quantification (LOQs) were 5 μg/kg （2 μg/kg for pork）and 10 μg/kg, respectively. The average recoveries of tulathromycin and its metabolites under different spiked levels were 72.6%-105.8% with intraday relative standard deviations (RSDs) of 0.5%-12.1% and interday relative standard deviations (RSDs) of 2.9%-8.1%. The method was easy, fast, highly sensitive and fine reproducibility, and was suitable for the determination of tulathromycin and its metabolites in pig tissue.