HLB净化/高分辨液质联用法快速筛查动物肝脏中45种兽药残留

Rapid Screening of 45 Kinds of Veterinary Drugs Residues in Animal Liver Using Prime HLB Purification/UHPLC-Q-Orbitrap HRMS

采用通过式固相萃取净化,基于超高效液相色谱-四极杆/静电场轨道阱高分辨质谱联用技术建立快速筛查和确证动物肝脏(猪肝、牛肝、羊肝、鸡肝、鸭肝和鹅肝)中45种兽药残留的方法。样品中药物用0.2%甲酸-80%乙腈水溶液提取,离心,固相萃取柱净化,氮吹后复溶。采用Waters Acquity BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm)分离,以含0.1%甲酸的乙酸铵(20 mmol/L)溶液-乙腈体系作为流动相梯度洗脱,在一级全扫描/数据依赖二级扫描监测模式下检测,基质匹配标准曲线外标法定量。结果表明:45种兽药在质量浓度1~2000μg/L范围内线性关系良好,相关系数大于0.9959;检出限0.5~20μg/kg,定量限2~50μg/kg。6种动物肝脏在3个添加水平下回收率为72.0%~112.2%,相对标准偏差为5.0%~10.5%。此方法前处理简单、通量高、准确可靠,适用于动物肝脏中45种兽药残留的快速筛查与确证。

A rapid screening and identification method for 45 veterinary drug residues in animal liver(pig liver,bovine liver,sheep liver,chicken liver,duck liver and goose liver)was established by using Prime HLB solid-phase extraction(SPE)purification and UHPLC-Q-Orbitrap high resolution mass spectrometry.The drugs were extracted with 0.2%formic acid and 80%acetonitrile aqueous solution,centrifuged,purified on Oasis Prime HLB solid phase extraction column,and redissolved after nitrogen blowing.The separation was performed on a Waters ACQUITY BEH C_(18) column(2.1 mm×100 mm,1.7μm).The mobile phase consisted of ammonium acetate(20 mmol/L)containing 0.1%formic acid and acetonitrile with gradient elution.The determination was performed in the first-stage full-scan/data-dependent two-stage scanmonitoring mode.The results showed that the linear relationships of 45 veterinary drugs were good in the concentration range of 1-2000μg/L,and the correlation coefficients were greater than 0.9959.The limits of detection were between 0.5 and 20μg/kg,and the limits of quantification were between 2 and 50μg/kg.The recoveries were 72.0%-112.2%with relative standard deviations(RSD)of 5.0%-10.5%at 3 supplemental levels.This method has the advantages of simple pretreatment,high throughput,accuracy and reliability,and is suitable for rapid screening and confirmative analysis of 45 veterinary drug residues in animal liver.