新型净化材料结合QuEChERS技术用于动物肌肉组织中β-受体激动剂的快速检测

Rapid determination of β-agonists in meat by QuEChERS technology with a new purification material

中文关键词:  QuEChERS  液相色谱-串联质谱法  β-受体激动剂  新型净化材料

英文关键词:QuEChERS  liquid chromatography-tandem mass spectrometry  β-agonists  new purification material

中文摘要:

      目的 建立食用肉类中9种β-受体激动剂残留的QuEChERS-液相色谱-三重四极杆质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)的检测方法。方法 样品经酶解后, 用1%氨化乙腈提取, 无水硫酸镁盐析后取乙腈相, 经新型净化材料分散固相萃取法净化。采用Kinetex 2.6μm F5(3.0 mm×50 mm, 2.6 μm)色谱柱, 经0.1%甲酸水溶液(A)和0.1%甲酸乙腈溶液(B)梯度洗脱, 于电喷雾正离子源(electrospray ionization, ESI+)和多反应监测模式(multiple reaction monitoring, MRM)下监测, 基质标准曲线定量。结果 9种β-受体激动剂在不同添加水平下, 相对回收率为70.2%~100.0%, RSD在1.0%~14.9% (n=3), 检出限为0.002~0.190 μg/kg, 定量限为0.01~0.76 μg/kg。结论 该方法操作简便、快速、净化效果好、准确性高, 适用于食用肉类中β-受体激动剂的残留确证。

英文摘要:

      Objective To establish a method for determination of 9 kinds of β-agonists residues in meat by QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Meat samples were extracted with 1% ammonia acetonitrile after enzymolysis, salted out by MgSO4, and then the organic phase were cleaned up by a new purification QuEChERS material. A Kinetex? 2.6μm F5 (3.0 mm×50 mm, 2.6 μm) column was used for separation, with a gradient elution program of 0.1% formic acid aqueous solution (A) and 0.1% formic acid in acetonitrile solution (B). ESI positive ion scan was used under multiple reaction monitoring (MRM) mode and quantified by matrix-matched external standard method. Results At different additional levels, the recoveries of 9 kinds of agonists were in the range of 70.2%-100.0% with the relative standard deviations of 1.0%-14.9% (n=3). The limits of detections were 0.002-0.190 μg/kg and the limits of quantitative were 0.01-0.76 μg/kg. Conclusion The method is simple, fast, accurate and has prominent effect in degreasing, which is suitable for detecting the agonists residues in meat.