超高效液相色谱-串联质谱法同时测定猪肉中 20种β-受体激动剂

Determination of 20 kinds of β-agonists residues in pork by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  β-受体激动剂  液相色谱串联质谱法  固相萃取

英文关键词:β-agonists  liquid chromatography-tandem mass spectrometry  solid-phase extraction

中文摘要:

      目的 建立猪肉中溴氯布特罗、非诺特罗、妥洛特罗、苯乙醇胺A等20种β-受体激动剂的超高效液相色谱-串联质谱检测方法。方法 猪肉样品经均质混匀并进行酶解和净化后, 选择 C18柱(2.1 mm×100 mm, 1.8 μm), 以0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱。正离子模式下, 以克伦特罗-D9为同位素内标, 采用多反应监测模式测定。结果 20种目标物在13 min内完成分离。 除多巴胺外, 其余19种β-受体激动剂在空白基质中的线性范围为0.05~10 μg/kg, 检出限为0.05 μg/kg, 相关系数大于0.998。在空白猪肉样品中添加浓度为0.5、1.0、5.0 μg/kg的待测物质时, 固相萃取净化法的回收率为82.3%~102.1%, 相对标准偏差为3.4%~7.2%。结论 本方法准确性高、操作简便, 可应用于猪肉中多种β-受体激动剂的定量检测。

英文摘要:

      Objective To establish a method for the determination 20 kinds of β-agonists residues in pork by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Being homogenized, hydrolyzed and purified, the pork samples were separated by a C18 column (2.1 mm×100 mm, 1.8 μm) utilizing gradient elution with water (0.1% formic) and methanol. Through positive ESI, the β-agonists were detected by tandem mass spectrometry in multiple reaction monitoring mode and calibrated by isotope internal standards, clenbuterol-D9. Results The analytes were completely separated in 13 minutes. Excluding dopamine, the detection limits of 19 kinds of β-agonists were 0.05 μg/kg, the linear ranges were 0.05~10 μg/kg and the correlation coefficients were more than 0.998. When spiked at 0.5, 1.0 and 5.0 μg/kg, the average recovery rates of 20 kinds of β-agonists were 82.3%~102.1% with relative standard deviations (RSD) of 3.4~7.2% when prepared by solid-phase extraction. Conclusion With the advantages of high sensitivity and simple analysis process, it is applicable for the detection of 20 kinds of β-agonists residues in pork.