液相色谱-质谱联用法测定猪肉组织中3种β-激动剂

Determination of 3 β-agonists in pig muscle by liquid chromatography and -tandem mass spectrometriy

目的建立高灵敏度的猪肉组织中沙丁胺醇、莱克多巴胺和克伦特罗同时测定的方法。方法样品匀浆好后用5%高氯酸溶液振荡提取,反相C18小柱净化浓缩,以乙腈-2mmol/L醋酸铵+0.1%甲酸水溶液为流动相进行梯度洗脱,通过液相色谱-质谱以MRM方式检测,以D3-沙丁胺醇为内标定量。结果测定3种β激动剂的方法的线性范围均为0.1～10.0μg/L,线性相关系数分别为0.9998、0.9991和0.9992,定量检出限分别为0.2μg/kg、0.3μg/kg及0.5μg/kg,回收率分别为89.9%～96.7%、84.9%～90.1%及88.4%～96.2%。结论方法简便,灵敏度好,选择性好,适合于猪肉组织样品中沙丁胺醇、莱克多巴胺及克伦特罗残留进行检测及结构确证。

Objective To develop a method for simultaneous determination of sabutamol, ractopamine and clenbuterol in pig muscle with high performance liquid chromatography mass spectrometry. Methods The pig muscle was hydrolyzed with 5% perchloric acid solution and then purified on C18 cartridge. D3-Sabutamol was used as internal standard,Multiple Reaction Monitor （MRM） method was applied for detection. Results The linear range of the three β-agonists were all found to be 0.1-10.0μg/ Land the correlation coefficient of the standard curve were 0.9998,0.9991 and 0.9992. The detection limit was 0.2p.g/kg,0.3μg/kg and 0.5μg/kg. The recoveries of sabutamol for the spiked samples ranged from 89.9% to 96.7%, that of ractopamine ranged from 84.9%-90.1% ,and that of clenbuterol ranged from 88.4% to 96.2%. Conculsion The HPLC-MS/MS method is suitable for detection of sabutamol,ractopamine and clenbuterol and structure confirmation with high sensitivity and specificity.