超高压液相色谱-串联质谱法同时测定婴幼儿配方乳粉中11种B族维生素  

Simultaneous Determination of 11 B Vitamins in Infant Formula by UPLC-MS/MS

作　　者：陈美君[1] 王旻[1] 亢美娟[1] 段奇慧 尚教文 单艺[1] 

机构地区：[1]东北农业大学黑龙江省乳品工业技术开发中心,黑龙江哈尔滨150028 [2]黑龙江民族职业学院,黑龙江哈尔滨150066

出　　处：《食品科学》2016年第4期144-153,共10页Food Science

摘　　要：目的：建立一种能够同时测定婴幼儿配方乳粉中11种B族维生素的超高压液相色谱-串联质谱法。方法：样品用0.1%甲酸溶液溶解,乙酸锌沉淀蛋白,滤液经ACQUITY UPLC HSS T3色谱柱分离,流动相为0.1%甲酸溶液和乙腈,梯度洗脱,采用电喷雾离子源正离子模式,多反应监测进行检测,分析时间12 min。结果：11种B族维生素在各自质量浓度范围内线性良好,R^2均大于0.99,加标回收率在85%-110%之间,相对标准偏差在1.03%-6.75%之间,VB1、VB2、烟酸、烟酰胺、泛酸（VB5）、吡哆醛、吡哆醇、吡哆胺、叶酸、游离生物素和VB12的定量下限分别为40.0、40.0、30.0、30.0、50.0、0.9、1.2、1.2、2.0、2.0、0.2μg/100 g,与国家标准比较,部分维生素定量限提高了7.7%-60%。结论：该法具有灵敏度高、前处理操作简单快速、分析时间短的特点,而且具有良好的精密度和准确性,可以应用于婴幼儿配方乳粉中11种B族维生素的同时测定。Objective： To establish a method for the simultaneous determination of 11 B vitamins in infant formula by ultrapressure liquidchromatography-tandem mass spectrometry（UPLC-MS/MS）. Methods： The samples were dissolved in 0.1%formic acid and then added with xinc acetate to precipitate the proteins. Then the filtrate was separated by an ACQUITY UPLC HSS T3 column through gradient elution using 0.1% formic acid and acetonitrile as the mobile phase. Mass spectral acquisition was done in the positive ion mode by applying multiple reaction monitoring and the analysis was completed in 12 min. Results： High correlation coefficients（R^2〉0.99） for 11 B vitamins in their linear ranges were obtained. The spiked recovery rates and accuracy（expressed as relative standard deviation,RSD） were determined to be in the ranges of 85%–110% and 1.03%–6.75%,respectively. The limits of quantitation（LOQs） for vitamin B1,vitamin B2,nicotinic acid,niacinamide,pantothenic acid,pyridoxal,pyridoxine,pyridoxamine,folic acid,vitamin H and vitamin B12 were 40.0,40.0,30.0,30.0,50.0,0.9,1.2,1.2,2.0,2.0,and 0.2 μg/100 g,respectively,an increase by 7.7% to 60% over those from the national standards of China. Conclusions： The method is characterized by high sensitivity,simple operation,fast analysis and short time. This method also has good precision and accuracy and can be applied to detect 11 B vitamins in infant formula.

关 键 词：B族维生素 婴幼儿配方乳粉 超高压液相色谱-串联质谱法 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]