羊奶及奶粉中27种β-受体激动剂类药物残留UPLC-MS/MS检测方法

刘洪斌; 李颖; 姚喜梅; 于雷; 蔡英华

doi:10.13386/j.issn1002-0306.2017.23.040

羊奶及奶粉中27种β-受体激动剂类药物残留UPLC-MS/MS检测方法

1. 中国动物疫病预防控制中心
2. 中国标准化协会

基金项目:

十二五国家科技支撑计划项目(2014BAD13B05)；兽药残留检测标准物质研制(2013FY113300-1)；

详细信息

作者简介:
刘洪斌 (1985-) , 男, 硕士, 工程师, 从事动物产品质量安全检测及风险评估方面的研究, E-mail:liuhongbin111@163.com。;

蔡英华 (1977-) , 男, 本科, 工程师, 从事动物产品质量安全检测及风险评估方面的研究, E-mail:caiyh@163.com。;

中图分类号: O657.63;TS252.7
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出版历程
- 收稿日期: 2017-03-28

Simultaneous determination of twenty-seven β-agonists residues in goat milk and powder using ultra performance liquid chromatography tandem mass spectrometry

China Animal Disease Control Center
China Association for Standardization

摘要

摘要: 采用超高效液相色谱串联质谱建立羊奶及奶粉中吡布特罗、丙卡特罗、瑞普特罗、克伦普罗、奥达特罗等27种β-受体激动剂类药物残留检测方法。样品经过1%甲酸乙腈提取、Oasis PRi ME HLB柱净化后,经Acquity UPLC BEH C18（100 mm×2.1 mm,1.7μm）分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,多通道MRM信号采集模式,27种β-受体激动剂类药物能在10.5 min内出峰完好,在1.0¹00.0μg/L浓度范围内,27种β-受体激动剂类药物线性良好,相关系数均在0.993以上;羊奶中最低定量限均低于0.5μg/kg,通过0.5、2.5、5.0μg/kg三个浓度的加标回收实验表明,回收率为65.7%¹19%,批内变异系数为0.79%¹0.4%,批间变异系数为2.13%¹5.7%。奶粉中最低定量限均低于2.0μg/kg,通过2.0、10.0、20.0μg/kg三个浓度的加标回收实验表明,回收率为60.5%¹09%,批内变异系数为1.91%¹2.4%,批间变异系数为3.06%¹7.2%。所建立方法为一种高通量检测羊奶及奶粉中β-受体激动剂类药物残留确证分析方法。
- 羊奶 /
- 奶粉 /
- β-受体激动剂类 /
- 残留 /
- UPLC-MS/MS
Abstract: A multiresidue method based on ultra performance liquid chromatography tandem mass spectrometry has been developed for the determination of twenty-seven β-agonists ( pyrbuterol, procaterol, reproterol, clenproperol, olodaterol. et al) residues in goat milk and powder.In this method, analytes were extracted by acidified acetonitrile, and purified by Oasis PRi ME HLB SPE column.twenty-seven β-agonists were analyzed by Acquity UPLC BEH C18 column ( 100 mm × 2.1 mm, 1.7 μm) using methanol and 0.1% formic acid as the mobile phases.The signals are acquired through the multi-channel MRM mode.All analytes could be well-separated by a gradient program during 10.5 minutes.The calibration curves of twenty-seven β-agonists were linear in a concentration range of 1.0¹00.0 μg/L ( r > 0.993) , and the limits of quantitation were all less than 0.5 μg/kg in goat milk.The recoveries of 0.5, 2.5, 5.0 μg/kg fortified samples ranged from 65.7% ¹19%, with the intra-assay coefficient of variation was 0.79% ¹0.4% and the inter-assay coefficient of variation was 2.13% ¹5.7%.The limits of quantitation were all less than 2.0 μg/kg in milk powder.The recoveries of 2.0, 10.0, 20.0 μg/kg fortified samples ranged from 60.5% ¹09%, with the intra-assay coefficient of variation was 1.91% ¹2.4% and the inter-assay coefficient of variation was 3.06% ¹7.2%.The method was established as a high-throughput method for confirmation of β-agonists residues in goat milk and powder.
- goat milk /
- milk powder /
- β-agonists /
- residues /
- UPLC-MS/MS

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