高效液相色谱-串联质谱法测定生乳中加米霉素残留量

Determination of residual levels of gamithromycin in raw milk by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  加米霉素  液相色谱串联质谱法  EMR净化柱  生乳

英文关键词:gamithromycin  high performance liquid chromatography-tandem mass spectrometry  EMR-Lipid through type purification column  raw milk

中文摘要:

      目的 建立以基质外标法定量, 通过式净化柱(EMR-Lipid)结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定生乳中加米霉素残留量的分析方法。方法 样品经酸性乙腈提取后, 由EMR-Lipid通过式净化柱净化, 通过BEH C18色谱柱进行梯度洗脱, 电喷雾正离子多反应模式进行检测, 基质外标法定量。结果 加米霉素在0.5~20.0 ng/mL质量浓度范围内呈现良好线性关系, 线性相关系数大于0.99; 检出限(limit of detection, LOD)为0.5 μg/kg; 定量限(limit of quantification, LOQ)为1.0 μg/kg; 加米霉素在生乳中表现为基质增强效应, 经基质空白曲线校正后, 加米霉素在不同添加浓度平均回收率为74.0%~77.0%, 测定结果的相对标准偏差(relative standard deviation, RSD)为3.92%~4.57%。结论 该方法准确、灵敏、稳定、简单易操作, 可以用于生乳中加米霉素残留量快速测定及定量分析, 为生乳中加米霉素残留监控提供技术支持。

英文摘要:

      Objective To establish an analytical method for the determination of gamithromycin residues in raw milk based on matrix external standard method combined with through type purification column (EMR-Lipid) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acid acetonitrile, purified by the EMR-Lipid through type purification column, gradient eluted through a BEH C18 chromatographic column. Detection was carried out in the electrospray positive ion multiple reaction mode, and quantification was performed using the matrix external standard method. Results Calibration curves were linear in the range of 0.5–20.0 ng/mL with correlation coefficients more than 0.99. The limit of detection (LOD) was 0.5 μg/kg, limit of quantification (LOQ) was 1.0 μg/kg. Gamithromycin showed a matrix enhancement effects in raw milk. After matrix blank curve correction, the average recoveries of gamithromycin at different spiked concentrations ranged from 74.0% to 77.0%, and the relative standard deviations (RSD) of the determination results were from 3.92% to 4.57%. Conclusion This method is accurate, sensitive, stable, simple, and easy to operate, it can be used for the rapid determination and quantitative analysis of gamithromycin residues in raw milk, providing technical support for monitoring the residual amount of gamithromycin in raw milk.