超高效液相色谱-四极杆飞行时间质谱快速筛查与确证生鲜牛乳中80种抗生素和激素

采用超高效液相色谱-四极杆飞行时间高分辨质谱(UHPLC-QTOF MS)技术建立了生鲜牛乳中80种抗生素和激素的快速筛查方法。牛乳样品经含1%乙酸的乙腈溶液提取,采用QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)方法净化。目标药物经Agilent ZORBAX SB C₁₈色谱柱(3. 0 mm×100 mm,1. 8μm)分离,以乙腈-0. 1%甲酸水溶液为流动相进行梯度洗脱,使用Dual AJS ESI源,在正离子模式下进行数据采集,基质匹配标准曲线法定量。结果表明,80种抗生素和激素类药物在各自的浓度范围内线性关系良好(r^2≥0. 990 0),其定量下限(LOQ,S/N=10)为5～100μg/kg。LOQ加标水平下,80种兽药中23种兽药的回收率为50. 2%～59. 7%,相对标准偏差为1. 1%～13. 0%;其余57种兽药的回收率为61. 7%～119%,相对标准偏差为0. 3%～19. 0%。结合精确分子质量数、保留时间、同位素丰度和二级特征碎片离子对目标化合物进行快速筛查与确证。该方法快速简便、准确、灵敏,适用于牛乳中抗生素和激素类药物残留的高通量筛查与定性鉴定。

Rapid Screening and Confirmation of 80 Antibiotic and Hormone Residues in Raw Milk by Ultra Performance Liquid Chromatography-Quadrupole Time of flight Mass Spectrometry

A comprehensive analytical method was established for the rapid screening of 80 kinds of antibiotics and hormones in raw milk by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UHPLC-QTOF MS).The milk samples were extracted with acetonitrile containing 1%acetic acid.The extracts were cleaned up through QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)method.80 target compounds were separated on an Agilent ZORBAX SB C 18 column(3.0 mm×100 mm,1.8μm)by gradient elution using acetonitrile-0.1%formic acid as mobile phases,and detected by MS under Dual AJS ESI^+mode.The analytes were quantified by the matrix-matched calibration standards.As a result,the calibration curves of 80 target compounds were linear in the certain concentration with their correlation coefficients not less than 0.990 0.The limits of quantitation(LOQ,S/N=10)for the compounds in milk were in the range of 5-100μg/kg.The average recoveries for 23 drugs in milk at LOQ spiked levels ranged from 50.2%to 59.7%with their relative standard deviations(RSDs)of 1.1%-13.0%,while those for the other 57 drugs ranged from 61.7%to 119%with their RSDs of 0.3%-19.0%.The screening and confirmation on the analytes were performed by using precision mass,retention time,isotopic abundance and two-stage ion mass spectra.The method could be applied in the high-throughput screening and identification of antibiotics and hormones in raw milk due to its characteristics of rapidness,simplicity,accuracy and sensitivity.