高效液相色谱-高分辨质谱法测定乳粉中的牛磺酸

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0.45μm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0.5~10μg/L范围内线性良好(r=0.9998),检出限(limit...

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Published in食品安全质量检测学报 Vol. 8; no. 6; pp. 2086 - 2090
Main Author 张婷 陈雷 刘芸 丁涛 张睿 吴斌 沈崇钰 邓晓军 伊雄海 郭德华
Format Journal Article
LanguageChinese
Published 江苏出入境检验检疫局动植物与食品检测中心,南京210001 2017
中国药科大学工学院,南京211198%江苏出入境检验检疫局动植物与食品检测中心,南京,210001%上海出入境检验检疫局,上海,200000
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ISSN2095-0381

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Summary: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0.45μm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0.5~10μg/L范围内线性良好(r=0.9998),检出限(limit of detection,LOD)为0.2μg/kg。分别在样品中添加牛磺酸标准溶液2、5、10μg/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。
Bibliography: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 gm, 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 ratesof 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 accu
ISSN:2095-0381