超高效液相色谱-电喷雾串联质谱法同时测定猪肉中4种β-受体激动剂类药物残留

Simultaneous determination of 4 kinds of β-agonist residues in pork by ultra performance liquid chromatography-electrospray tandem mass spectrometry

中文关键词:  克伦特罗  莱克多巴胺  沙丁胺醇  特布他林  β-受体激动剂  超高效液相色谱-串联质谱

英文关键词:clenbuterol  ractompamine  salbutaline  terbutaline  β-agonist  ultra performance liquid chromatography-

中文摘要:

      目的 建立超高效液相色谱-电喷雾串联质谱法检测猪肉组织中克伦特罗、莱克多巴胺、沙丁胺醇和特布他林4种β-受体激动剂类药物残留。方法 样品用β-盐酸葡萄糖醛苷酶酶解, 经乙酸乙酯提取, 经MCX固相萃取小柱净化, 以Eclipse Plus C18色谱柱(2.1 mm×50 mm, 1.8 μm)分离, 以0.1%甲酸、2 mmol/L乙酸铵水溶液和0.1%甲酸乙腈溶液为流动相进行梯度洗脱。质谱分析以电喷雾为离子源, 采用多反应监测, 以正离子扫描模式进行检测。结果 4种β-受体激动剂类药物在0.5~50 ng/mL浓度范围内呈良好的线性关系, 相关系数r2≥0.9973, 方法定量限为0.1 μg/kg, 平均回收率为65.5%~109.1%, 相对标准偏差为6.6%~15.4%(n=6)。结论 本方法具有定量限低、准确度高及稳定性好等特点, 可以满足样品检测的要求。

英文摘要:

      Objective To establish a method for the determination of 4 kinds of β-agonist (including clenbuterol, ractompamine, salbutaline, and terbutaline) residues in pork muscle by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were processed for enzymolysis with β-hydrochloride glucose aldehyde enzyme, extracted with ethyl acetate, cleaned up by MCX solid phase extraction(SPE), and separated by the column of Eclipse Plus C18 (2.1 mm×50 mm, 1.8 μm) using 0.1% formic acid, 2 mmol/ L ammonium acetate and 0.1% formic acid in acetonitrile as the mobile phase for gradient elution. The positive electrospray ionization mode and the multiple reaction monitoring mode were used for the detection. Results Four kinds of β-agonist residues had good linear relationships in the range of 0.5~50 ng/mL, with correlation coefficients of no less than 0.9973, and the limits of quantitation were 0.1 μg/kg. The average recoveries were 65.5%~109.1%, and the relative standard deviations were 6.6%~15.4% (n=6). Conclusion This method has low limit of quantitation, high accuracy and good stability, can meet the demand of the determination of samples.