UPLC-IDMS法测定配方奶粉中的生物素含量.pdfVIP

136 2015, Vo1.36, No.04 层面露盟军 ※成分分析 UPLC-IDMS法测定配方奶粉中的生物素含量 梁敏慧1 ，崔亚娟2.* ，叶润2 ，李全霞2 ，陈兆天2 ，李菁菁2，李东2 (1北京工业大学生命科学与生物工程学院，北京 100124; 2北京市营养源研究所，北京 l(削69) 摘 要z 建立一种超高效液相色谱.同位素稀释质谱法测定配方奶粉中生物素含量的方法。样品中加入生物素-D 2 作为同位素内标，经水超声提取后，以含体积分数 0.1% 甲酸的10 mmolfL乙酸镀溶液和乙庸作为流动相进行梯度 洗脱，采用电喷雾正离子模式、多反应监测方式进行定性定量分析。结果表明:生物素在1~50ng/mL范围内线性 关系良好，线性范围内对己知生物素含量样品3 个标准添加水平的平均回收率为89.6%~93.1 %，相对标准偏差为 1.71%~4.33%。方法检出限为0.6μg/l00 g ，定量限为1.5μg/l00 g，该方法具有灵敏度高、重复性好、分析时间短 等优点，可以满足配方奶粉中生物素含量的测定要求。 关键词:生物素:超高效液相色谱.同位素稀释质谱:奶粉 Determination of Biotin in Milk Powder by Using Ultra Performance Liquid Chromatography-Isotope Dilution Mass Spectrometry 2 2 2 2 2 2 LIANG Minhui\ CUI Y句uan .* ， YE Run , LI Quanxia , CHEN Zhaotian , LI Jingjing , LI Dong (1. College of Life Science and Bioengineering, Beijing University of Technology, Beijing 1∞124， China; 2. Beijing Research Institute for Nutritional Resources , Beijing 1α泊69， China) Abstract: An ultra performance liquid chromatography-isotope dilution mass spectrome町Y (UPLC-IDMS) method has been developed for the determination of biotin in milk powder. After spiking biotin-D2 as an intemal stand缸址， samples were extracted with water. The mobile phase consisted of 10 mmo lfL arnmonium acetate with 0.1 % formic acid and acetoni回le. The biotin was identified under multiple-reaction monitoring (MRM) mode and quantified by an intemal standard method. ηle results showed a good linear calibration in the range of 1-50 ng/mL, the recoveries at three spiked levels a