高压液相色谱-串联质谱法测定婴幼儿配方奶粉中7种B族维生素含量

[目的]建立一种高压液相色谱-串联质谱同时测定婴幼儿配方奶粉中7种B族维生素(核黄素、硫胺素、吡哆醇、吡哆胺、吡哆醛、烟酸、烟酰胺)含量的方法。[方法]样品用0.1%甲酸溶液溶解后,加入一定体积的正己烷,经过超声、离心、过滤处理。用0.1%甲酸-甲醇为流动相(梯度洗脱),Eclipse Plus C18色谱柱为分析柱,对滤液进行分离。采用电喷雾正离子模式,多重反应监测(MRM)对7种B族维生素进行检测。[结果]7种B族维生素在5 min内能较好分离,在一定的浓度范围内线性良好,相关系数(R2)均大于0.99,样品加标回收率(3个加标水平)为75.25%~107.65%,相对标准偏差在3%以下。[结论]该方法具有操作简单、分离度好、灵敏度高、检测速度快等优点,可用于婴幼儿配方奶粉中B族维生素含量的检测。

Simultaneous Determination of 7 B Vitamins in Infant Formula by HPLC-MS-MS

[Objective]A high-pressure liquid chromatography and tandem mass spectrometry method for determination of 7 B vitamins(thia-mine,riboflavin,pyridoxine,pyridoxal,pyridoxamine,nicotinic acid and nicotinamide) in infant formula was studied.[Method]The samples were dissolved by 0.1% formic acid solution and added certain volume of hexane. After ultrasonic,centrifugal and filter treatment,the filter liquor was separated by an Eclipse plus C18column through gradient elution using 0.1% formic acid and methanol as the mobile phase. Mass spectral acquisition was done in the positive ion mode by applying multiple reaction monitoring. 7 B vitamins could be separated in 5 minutes. Good linearitis in certain concentration range,the correlation coefficients(R2) were greater than 0.99,the recoveries(three spiked levels) in 75.25% -107.65%, the relative standard deviation was below 3%. [Conclusion]The method is characterized by simple operation, good separation,high sensitivity and fast detection speed. This method can be applied to detect 7 B vitamins in infant formula.