液相色谱-串联质谱法检测猪尿中26种β2-受体 激动剂类药物残留

Simultaneous determination of 26 kinds of β2-agonist residues in swine urine samples by liquid chromatography-tandem mass spectrometry

中文关键词:  β2-受体激动剂  液相色谱-串联质谱法  猪尿  残留

英文关键词:β2-agonist  liquid chromatography-tandem mass spectrometric  swine urine  residues

中文摘要:

      目的 建立了一种在猪尿中检测26种β2-受体激动剂兽药残留的液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法 样品经β-葡萄糖苷酸酶/芳基硫酸酯酶酶解后, 用正丁醇及甲基叔丁基醚混合液萃取, 过混合阳离子(MCX)固相萃取柱净化。采用0.1%甲酸溶液(A) 和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱, 质谱(ESI+)采用多离子检测模式(MRM)对β2-受体激动剂的定量离子和定性离子进行监测。结果 本方法在15 min内完成26种目标化合物的分析, 实现高通量检测, 可有效地提高β2-受体激动剂检测效率。26种β2-受体激动剂在5、10和20 μg/kg添加水平的回收率为65.0%~105.3%, 相对标准偏差小于11.5%(n=6), 方法检出限为0.04~1.02 μg/kg。结论 该方法快速、准确、灵敏, 适合测定猪尿中的β2-受体激动剂类药物残留。

英文摘要:

      Objective To establish a sensitive liquid chromatography-tandem mass spectrometric (LC–MS/MS) method for simultaneous determination of 26 kinds of β2-agonist residues in swine urine samples. Methods Swine urine samples were extracted with N-butyl alcohol and methyl tert-butyl ether, purified by the solid phase extraction. And then the 26 kinds of β2-agonist residues in the extracts were separated on a reversed phase using a gradient elution program of 0.1% formic acid aqueous solution (A) and 0.1% formic acid in acetonitrile solution (B). Multiple reaction monitoring (MRM) with positive polarity was selected to monitor qualitative and quantitative ion. Results Based on the optimized method, 26 kinds of β2-agonists could be analyzed in 15 min, and the method realized high-throughput detection and brings a higher efficiency and benefits to testing β2-agonists. The recoveries ranged from 65.0% to 105.3% for the 26 kinds of β2-agonist residues with three spiked levels of 5, 10 and 20 μg/kg. The relative standard deviations (RSDs) were less than 11.5%(n=6). The limits of detection (LOD) for the 26 kinds of β2-agonists were 0.04~1.02 μg/kg. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for detecting β2-agonist residues in swine urine samples.