超高效液相色谱-串联质谱法测定牛肉中9种β-受体激动剂

Determination of 9 kinds of β-agonists in beef by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  牛肉  超高效液相色谱-串联质谱法  多级反应监测  增强子离子扫描  β-受体激动剂  内标法  固相萃取

英文关键词:beef  ultra performance liquid chromatography-tandem mass spectrometry  multiple reaction monitoring  enhanced product ion  β-agonist  internal standard  solid phase extraction

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定牛肉中特布他林、西马特罗、沙丁胺醇、菲诺特洛、氯丙那林、莱克多巴胺、克伦特罗、妥布特罗、喷布特罗9种β-受体激动剂的分析方法。方法 样品经过酸性酶解, 经MCX固相萃取柱净化, 以甲醇-0.1%甲酸水为流动相进行梯度洗脱, 在碰撞能量(collision energy, CE)为(35±14) eV条件下, 采用多级反应监测触发增强子离子扫描检测模式(multiple reaction monitoring-information dependent acquisition-enhanced product ion, MRM-IDA-EPI)进行定性分析并建立子离子谱库, 同位素内标法定量。结果 9种β-受体激动剂在0.2~25.0 μg/L的检测浓度下呈线性关系, 加标回收率为82.3%~105.2%, 相对标准偏差小于5.4%, 方法检出限为0.028~0.075 μg/kg, 样品谱库匹配度高于82%。结论 该方法操作简便, 净化效果好, 灵敏度高, 通过谱库比对, 能有效的降低质谱定性过程中的基质干扰, 大大提高定性准确性, 可快速、准确的的测定牛肉中的9种β-受体激动剂。

英文摘要:

      Objective To establish an analytical method for the determination of 9 kinds of β-agonists (terbutaline, cimatero, salbutamol, fenotol, chloroproprine, lectadine, clentrol, tobuterol, and spurtro) in beef by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were enzyme hydrolyzed, extracted and cleaned up on a MCX SPE cartridge, and then separated by using elution with methanol and water (containing 0.1% formic acid) as mobile phase. Under the condition of collision energy (CE) of (35±14) eV, qualitative and quantitative analysis were carried out using predictive multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) scanning. The ion spectrum library was established and the isotope internal standard method was used for quantitative analysis. Results The mass concentration of 9 kinds of β-agonists showed good linearity in the range of 0.2–25.0 μg/L with peak area. The recoveries were 82.3%–105.2% and the relative standard deviations were less than 5.4%. The limits of detection of 9 kinds of β-agonists were 0.028–0.075 μg/kg. Compared with the secondary spectrum library, the matching degrees were higher than 82%. Conclusion The method is easy to operate and has good purification effect and high sensitivity. Through the comparison of spectrum library, it can effectively reduce the matrix interference in the qualitative process of mass spectrometry, and greatly improves the qualitative accuracy. This method can be used for the rapid and accurate determination of 9 kinds of β-agonists in animal-derived foods such as beef.