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

作　　者：张婷[1,2] 陈雷[1] 刘芸[1] 丁涛[1] 张睿[1] 吴斌[1] 沈崇钰[1] 邓晓军[3] 伊雄海[3] 郭德华[3] ZHANG Ting CHEN Lei LIU Yun DING Tao ZHANG Rui WU Bin SHEN Chong-Yu DENG Xiao-Jun YI Xiong-Hai GUO De-Hua(Animal, Plant and Food Inspection Center, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China College of Engineering, China Pharmaceutical University, Nanjing 211198, China Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200000, China)

机构地区：[1]江苏出入境检验检疫局动植物与食品检测中心,南京210001 [2]中国药科大学工学院,南京211198 [3]上海出入境检验检疫局,上海200000

出　　处：《食品安全质量检测学报》2017年第6期2086-2090,共5页Journal of Food Safety and Quality

基　　金：江苏出入境检验检疫局科技计划项目(2015KJ29);上海长三角科技合作项目(15395810100和16395810100)~~

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0.45μm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。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 accurate, simple and rapid, and the precision, accuracy and sensitivity can meet the requirements of the determination of taurine in milk powder.

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 

分 类 号：O657.63[理学—分析化学] TS252.51[理学—化学]