液相色谱-串联质谱法检测饲料中26种β2-受体激动剂类药物残留

Simultaneous determination of 26 β2-agonist residues in feed by liquid chro-matography-tandem mass spectrometry

中文关键词:  β2-受体激动剂  液相色谱-串联质谱法  饲料  残留

英文关键词:β2-Agonist  high performance liquid chromatography-tandem mass spectrometry  feed  residues

中文摘要:

      目的 建立一种饲料中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 样品经盐酸甲醇提取液提取, 醋酸铅沉淀蛋白后, 过混合阳离子(MCX)固相萃取柱净化。采用0.1%甲酸(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种目标化合物的分离分析。26种β2-受体激动剂在20、50和100 μg/L添加水平的回收率为71.9%~102.9%, 相对标准偏差小于11.8% (n=6), 方法定量限为10 μg/kg。结论 该方法快速、准确、灵敏, 适合测定饲料中的β2-受体激动剂类药物残留。

英文摘要:

      Objective To determination of 26 β2-agonist residues in feed samples by liquid chromatography -tandem mass spectrometric (LC–MS/MS). Methods Feed samples were extracted with muriatic acid and methanol solution. And then the 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). Using LC–MS/MS (ESI+) with multiple reactions monitoring (MRM), identification of the major components of the 26 kinds of β2-agonist residues was performed based upon the intensities of fragments. Results The recoveries were ranged from 71.9% to 102.9% for the 26 kinds of β2-agonist residues with 3 spiked levels of 20, 50 and 100 μg/kg. The relative standard deviations (RSDs) were less than 11.8% (n=6), and the limits of quantitation (LOQ) for the 26 kinds of β2-agonists were 10 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting β2-agonist residues in feed samples.