HLB固相萃取小柱应用于液相色谱-串联质谱法 测定兽药残留的性能研究

Study on the Performance of HLB Solid Phase Extraction for the Determination of Veterinary Drug Residues by Liquid Chromatography Tandem Mass Spectrometry

以国标GB 31658.17—2021《食品安全国家标准动物性食品中四环素类、磺胺类和喹诺酮类药物残留量的测定液相色谱-串联质谱法》为前处理方法,采用几种不同类型萃取柱进行样品加标回收试验,以液相色谱-串联质谱法对猪肉中的四环素类、磺胺类和喹诺酮类药物进行测定,外标法定量。结果表明,对于7种药物回收率最高的为单体比例为13/8的自制HLB萃取柱,3种不同添加质量浓度(10,20,50 ng/mL)的回收率为62.2%~101.4%,相对标准偏差(RSD)均小于7%,且高于其他商品化HLB萃取柱。研究表明,自制HLB固相萃取柱相较于其他商品柱有更好的性能,可以作为商品HLB小柱的替代品。

This article used the national standard GB 31658.17—2021《National food safety standard Determination of tetracyclines,sulfonamides and fluoroquinolones residues in animal derived food by liquid chromatography-tandem mass spectrometric method》as the preprocessing method.Several different types of extraction columns were used for sample addition and recovery experiments.The tetracycline,sulfonamide,and quinolone drugs in pork were determined by liquid chromatography-tandem mass spectrometry,and quantified by external standard method.The results showed that the self-made HLB extraction column with a monomer ratio of 13/8 had the highest recovery rates for the seven drugs.The recovery rates for the three different added concentrations(10,20,50 ng/mL)ranged from 62.2%~101.4%,and the relative standard deviation(RSD)was less than 7%,which was higher than other commercial HLB extraction columns.This study indicates that self-made HLB solid-phase extraction columns had better performance compared to other commercial columns and could be used as a substitute for commercial HLB small columns.