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超高压液相色谱-串联质谱法同时测定婴幼儿配方奶粉中11种B族维生素

陈美君1,王旻2,亢美娟2,段奇慧2,尚教文2,单艺1   

  1. 1. 黑龙江省乳品工业技术开发中心
    2. 国家乳制品质量监督检验中心
  • 收稿日期:2015-03-28 修回日期:2015-12-18 出版日期:2016-02-25 发布日期:2016-02-23
  • 通讯作者: 王旻 E-mail:wm0987@sina.com

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

Mei-jun CHEN 2, 2, 2,   

  • Received:2015-03-28 Revised:2015-12-18 Online:2016-02-25 Published:2016-02-23

摘要: 目的 建立一种能够同时测定婴幼儿配方奶粉中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%甲酸水溶解,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%甲酸水溶液和乙腈,梯度洗脱,采用ESI+离子源、MRM模式进行检测,分析时间12min。结果11种B族维生素在各自浓度范围内线性良好,R2均大于0.99,加标回收率在85%~110%之间,相对标准偏差(RSD)在1.03%~6.75%,维生素B1、维生素B2、烟酸、烟酰胺、泛酸(B5)、吡哆醛(PL)、吡哆醇(PN)、吡哆胺(PM)、叶酸、生物素H和维生素B12的定量下限(LOQ)分别为40.0、40.0、30.0、30.0、50.0、0.9、1.2、1.2、1.2、2.0、2.0μg/100g,与国家标准比较,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奶粉中11种B族维生素的同时测定。

关键词: B族维生素, 婴幼儿配方乳粉, 超高压液相色谱质谱法

Abstract: Objective Establish a can simultaneously determination of 11 kinds of B vitamins in infant formula by ultra-pressure liquid-chromatography tandem mass spectrometry (UPLC-MS/MS).Methods The sample used 0.1 % formic acid to dissolved for extraction, zinc acetate precipitate protein. Then the filtrate was separated by an ACQUITY UPLC HSS T3 column, and gradient elution was performed with 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, analysis time 12min. Results The 11 kinds of B vitamins in lineal range had got high correlation coefficients(R2>0.99) .The spiked recovery rates were determined between 85%~110%,accuracy between 1.03 %~6.75 %. Vitamin B1, Vitamin B2,Nicotinic acid, niacinamide, pantothenic acid, pyridoxal, pyridoxine, pyridoxamine, folic acid, Vitamin H and vitamin B12 of the lower limit of quantitation (LOQ) were 40.0, 40.0, 30.0, 30.0, 50.0, 0.9, 1.2, 1.2, 1.2, 2.0, 2.0μg/100g. Comparison with national standards, the limit of quantification increase by 7.7% to 60%.Conclusion The method has high sensitivity, simple operation,fast analysis short time characteristics, but also has good precision and accuracy that can be applied to infant formula in 11 kinds of B vitamins detection.

Key words: B vitamins, Infant formula milk powder, Ultra Pressure Liquid Chromatography-Mass spectrometry/Mass spectrometry

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