高效液相色谱-高分辨质谱法测定乳粉中的牛磺酸

Determination of taurine in milk powder by high performance liquid chromatography-high resolution mass spectrometry

中文关键词:  高效液相色谱-四极杆/静电场轨道阱质谱法  高分辨质谱法  牛磺酸  乳粉

英文关键词:high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry  high resolution mass spectrometry  taurine  milk powder

中文摘要:

      目的 建立高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry, HPLC-Q/ORBITRAPMS)测定乳粉中牛磺酸。方法 奶粉样品用水溶解, 加乙酸锌沉淀蛋白, 经离心、过0.45 μm粒径的微孔膜过滤后, 采用HPLC-Q/ORBITRAPMS进行分析检测。质谱采用正离子模式分析, 同位素内标法定量。结果 该方法在0.5~10 μg/L范围内线性良好(r=0.9998), 检出限(limit of detection, LOD)为0.2 μg/kg。分别在样品中添加牛磺酸标准溶液2、5、10 μg/kg水平上进行添加回收率实验, 方法回收率在79.9%~94.4%范围内, 相对标准偏差在4.7%~6.9%范围内(n=5)。结论 该方法具有准确度高、简单、快速等特点, 精密度、准确度和灵敏度均满足乳粉中牛磺酸的检测要求。

英文摘要:

      Objective To establish a method for the determination of taurine in milk powder by high performance liquid chromatography Quadrupole/electrostatic field orbitrap high resolution mass spectrometry (HPLC-Q/ORBITRAPMS). Methods The milk powder samples were dissolved in deionized water. Subsequently, aqueous solution of zinc acetate was used to precipitate protein. After centrifugation, the final aqueous solution was filtered by a polytetrafluoroethylene (PTFE) membrane with pore size of 0.45 μm, then analyzed by HPLC-Q/ORBITRAPMS in positive ionization mode, and the isotope internal standards were used for quantitative analysis. Results Internal standard method was used to determine the taurine contents with a good linear relationship in the range of 0.5~10 μg/L (r=0.9998). The limit of detection (LOD) was 0.2 μg/kg. The recovery rates of taurine at three levels of 2, 5, 10 μg/kg were from 79.9% to 94.4% with the relative standard deviations (RSDs) of 4.7%~6.9% (n=5) in milk powder. Conclusion This method is accurate, simple and rapid, and the precision, accuracy and sensitivity can meet the requirements of the determination of taurine in milk powder.