| 摘要: |
| 建立了高选择性MRM3液质联用技术检测猪肝脏等复杂动物性食品中克仑特罗、莱克多巴胺和沙丁胺醇三种β-受体激动剂残留的新方法。猪肝脏样品经酶解后用乙酸乙酯和叔丁基甲醚萃取,MCX固相萃取柱净化,0.1%甲酸乙腈溶液和0.1%甲酸溶液为流动相,Phenomenex F5(50×3.0mm,2.6μm)色谱柱进行梯度洗脱,在电喷雾正离子源下,采用三级质谱多反应监测模式(MRM3)检测。结果表明：克仑特罗、莱克多巴胺和沙丁胺醇在系列浓度范围内均呈现良好线性关系,相关系数R2均大于0.99,猪肝脏组织中的定量限均为0.5μg/kg。从0.5、2和10μg/kg三个添加浓度检测结果可以看出,三种药物的回收率范围为89.7%~102.1%,批内、批间相对标准偏差均小于20％。该方法稳定性好,选择性强,灵敏度高,定性定量更加准确。 |
| 关键词: MRM3 液质联用技术 复杂动物性食品 β-受体激动剂 残留 |
| DOI： |
| 投稿时间：2021-04-13修订日期：2021-05-06 |
| 基金项目: |
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| Determination of β-agonists residue in complex animal derived food by LC-MS/MS/MS in high selectivity MRM3 |
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| (China Institute of Veterinary Drug Control) |
| Abstract: |
| A novel method based on LC-MS/MS/MS in high selectivity MRM3 was established for the determination of clenbuterol、ractopamine and salbutamol residues in complex animal derived food. The pig liver sample was extracted by ethyl acetate and tert-butyl methyl ether after enzymolysis, and purified on a mixed-mode cation exchange solid phase extraction column(MCX). A F5 chromatography column was used with acetonitrile(0.1% formic acid) and water(0.1% formic acid) as mobile phases in a gradient elution. Ionization was performed using an electrospray positive ion source(ESI+),and detection was achieved by MS/MS/MS in multiple reaction monitoring(MRM3) mode. The linearity for clenbuterol、ractopamine and salbutamol was good between serial concentrations, and the correlation coefficient was R2＞0.99. The limits of quantification of clenbuterol、ractopamine and salbutamol in pig liver tissue was 0.5μg/kg, The average recoveries from spiked pig liver tissues at three concentrations of 0.5, 2 and 10μg/kg ranged 89.7%~102.1%. The intra- and inter-batch variation coefficients were both less than 20%. This method was good stability, high sensitivity, qualitative and qualitative more accurately . |
| Key words: MRM3 LC-MS/MS/MS complex animal derived food β-agonists residue |
