| 猪肝中β-受体激动剂多残留的样品前处理方法比较及同时检测 |
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| 基金项目:国家自然科学基金资助项目（31072166） |
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| 中文摘要:比较了乙酸铵提取法（即农业部1025号公告-18-2008方法）、乙腈直接提取法及10%碳酸钠-乙腈溶液提取法对猪肝脏中9种β 受体激动剂残留的提取效果。结果表明，乙酸铵提取法对非诺特罗和喷布特罗等药物的回收率较低（小于20%）；乙腈直接提取法可有效提取出喷布特罗，其回收率达79%，但对非诺特罗的回收率仅为32%；而10%碳酸钠-乙腈溶液提取9种药物的效果明显好于其他两种方法，除了非诺特罗的回收率为72%外，其他8种药物的回收率均在80%以上。基于此，建立了猪肝脏中9种β-受体激动剂残留检测的高效液相色谱-串联质谱法。在优化条件下，9种药物在0.50~25 μg/kg范围内线性关系良好，相关系数（r）均大于0.99；在0.50、2.0、10 μg/kg 3个加标水平的回收率为71%~105%，相对标准偏差均小于15%；9种药物的检出限均达0.2 μg/kg。方法的准确度和精密度达到残留分析要求。 |
| 中文关键词:β-受体激动剂 前处理 猪肝脏 高效液相色谱-串联质谱 比较 |
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| Comparison of Pretreatment Methods of β-Agonists Residues in Pig Liver and Their Simultaneous Determination |
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| Abstract:Three extraction solvents such as ammonium acetate solution（used in No.1025-18-2008 Bulletin of the Ministry of Agriculture）,acetonitrile and acetonitrile-10% sodium carbonate solution were used to extract nine β-agonists residues in pig liver,respectively,and the extraction efficiencies of targeted compounds were compared.The experimental results revealed that the recovery of penbutolol increased to 79% and that for fenoterol was 32% when using acetonitrile as extraction solvent.The recoveries of the eight drugs（ractopamine,clenbuterol,salbutamol,terbutaline,cimaterol,clorprenaline,tulobuterol and penbutolol） were more than 80% except that 72% of recovery for fenoterol when using acetonitrile-10% sodium carbonate as extraction solvent.A liquid chromatography-tandem mass spectrometric method was established for the simultaneous determination of nine β-agonists residues in pig liver.Under the optimal conditions,the linear ranges of nine analytes were between 0.50 μg/kg and 25 μg/kg with correlation coefficients（r） more than 0.99.At the spiked levels of 0.50,2.0,10 μg/kg,the mean recoveries of nine β-agonists in pig liver ranged from 71% to 105%,with intra- and inter-RSD less than 15%.All the detection limits of nine β-agonists were 0.2 μg/kg.The method could meet the requirements for residue analysis on accuracy and precision. |
| Key Words:β-agonist pretreatment pig liver high performance liquid chromatography-tandem mass spectrometry comparison |
| 引用本文：刘敏,刘戎,王立琦,贺利民,贺倩倩,张高奎.猪肝中β-受体激动剂多残留的样品前处理方法比较及同时检测[J].分析测试学报,2012,31(3):290-295. |
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