| 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 |
| 点此下载全文 |
|
| 基金项目:上海市科技兴农项目(沪农科攻字(2016)，第4-5号) |
|
| 中文摘要: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，1.8 μm)分离，以乙腈-01% 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(r2≥0.990 0)，其定量下限(LOQ，S/N=10)为5~100 μg/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。 |
| 中文关键词:超高效液相色谱-四极杆飞行时间质谱(UHPLC-QTOF MS) 生鲜牛乳 抗生素 激素 快速筛查 |
| |
| Rapid Screening and Confirmation of 80 Antibiotic and Hormone Residues in Raw Milk by Ultra Performance Liquid Chromatography-Quadrupole Time of flight Mass Spectrometry |
|
|
| Abstract: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 C18 column(3.0 mm×100 mm，1.8 μm) by gradient elution using acetonitrile-01% 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 0990 0.The limits of quantitation (LOQ,S/N=10) for the compounds in milk were in the range of 5-100 μg/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. |
| Key Words:ultra performance liquid chromatography-quadrupole time of flight mass spectrometry (UHPLC-QTOF MS) raw milk antibiotics hormones rapid screening |
| 引用本文：贡松松,张婧，严凤，吴剑平,潘娟，顾欣.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[J].分析测试学报,2019,38(1):22-30. |
| 摘要点击次数: 2180 |
| 全文下载次数: 1219 |
| 查看全文 下载PDF阅读器 |
|
|
