Simultaneous determination of twenty-seven β-agonists residues in goat milk and powder using ultra performance liquid chromatography tandem mass spectrometry
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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。
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关键词:
- 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.-
Keywords:
- goat milk /
- milk powder /
- β-agonists /
- residues /
- UPLC-MS/MS
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