超高效液相色谱-同位素稀释质谱法测定配方奶粉中的泛酸.PDF

212 2014, Vol.35, No.08 食品科学 ※分析检测 超高效液相色谱-同位素稀释质谱法测定 配方奶粉中的泛酸 1 1 1 1 1 2 渠 岩 ，崔亚娟 ，李全霞 ，陈兆天 ，李 东 ，梁敏慧 （1.北京市营养源研究所，北京 100050 ；2.北京工业大学生命科学与生物工程学院，北京 100022 ） 摘  要：建立测定配方奶粉中泛酸的超高效液相色谱- 同位素稀释质谱方法。样品经乙酸铵溶液提取、三氯甲烷除 蛋白后，进行超高效液相色谱- 串联质谱分析，采用HSS T3液相色谱柱分离，以10 mmol/L乙酸铵溶液（含0.1% 甲 酸）和乙腈为流动相进行梯度洗脱，多反应监测模式，内标法定量。结果表明：方法定量限为0.040 mg/100 g ，线 性范围内低、中、高3 个标准添加水平的回收率为96.9%～104.3%，相对标准偏差为3.78%～5.04% 。该方法操作过 程简单、分析周期短、灵敏度高、重复性好，适用于奶粉中泛酸的测定。 关键词：泛酸；超高效液相色谱- 同位素稀释质谱方法；配方奶粉 Determination of Pantothenic Acid in Formula Milk Powder Using Ultra Performance Liquid Chromatography-Isotope Dilution Mass Spectrometry 1 1 1 1 1 2 QU Yan , CUI Ya-juan , LI Quan-xia , CHEN Zhao-tian , LI Dong , LIANG Min-hui (1. Beijing Research Institute for Nutritional Resources, Beijing 100050, China; 2. College of Life Science and Bio-engineering, Beijing University of Technology, Beijing 100022, China) Abstract: An ultra performance liquid chromatography-isotope dilution mass spectrometry (UPLC-IDMS) method has been developed for the determination for pantothenic acid (PA) in formula milk powder. Samples were extracted with ammonium acetate solution, and precipitated protein by adding chloroform for analyzing by UPLC-MS-MS. The analyte was separated using an HSS T3 column. The mobile phase consisted of 10 mmol/L ammonium acetate with 0.1% formic acid and acetonitrile. The PA was identified by multiple reaction monitoring (MRM) and quantified by internal standard method. The results showed that the limit of qu