摘要
目的使用两泵一阀的二维液相色谱系统,建立在线净化二维液相色谱法检测特殊医学用途配方食品中牛磺酸的分析方法。方法利用中心切割方法搭建在线二维液相色谱分离系统。以C18柱作为一维色谱柱、0.1%三氟乙酸和甲醇作为流动相对样品溶液进行初步分离净化,以五氟苯基(pentafluorophenyl,PFP)色谱柱作为二维色谱柱、0.1%甲酸和乙腈作为流动相进行二次分离。由牛磺酸衍生物在一维色谱上的保留时间确定阀切换时间,由C_(18)小柱作为富集柱捕获牛磺酸衍生物,二极管阵列检测器(diode array detector,DAD)进行检测,建立在线二维液相色谱分析方法。优化丹磺酰氯柱前衍生法前处理条件,并从多个方面对建立的方法进行方法学考察。结果牛磺酸衍生物在2.5~40.0μg/mL范围内具有良好线性关系,相关系数大于0.999;检出限为1.2 mg/100 g,定量限为4.0 mg/100 g;该方法回收率为95.28%~97.58%,相对标准偏差为0.56%~1.38%,可以满足特殊医学用途配方食品中牛磺酸的定量分析需要。结论本研究建立的方法自动化程度高、分析时间较短、准确度高、重复性好,适用于特殊医学用途配方食品中的牛磺酸检测。
Objective To establish an on-line two-dimensional liquid chromatography method for the determination of taurine in formula food for special medical purpose by using a two-dimensional liquid chromatography system.Methods The online two-dimensional liquid chromatography separation system was built by the central cutting method.A C_(18) column was used as the one-dimensional chromatographic column,and 0.1%trifluoroacetic acid and methanol were used as the mobile phases for preliminary separation and purification of the sample solution.A pentafluorophenyl(PFP)chromatographic column was used as the two-dimensional chromatographic column,and 0.1%formic acid and acetonitrile were used as the mobile phases for secondary separation.The valve switching time was determined by the retention time of taurine derivatives in one-dimensional chromatography.Taurine derivatives were captured by a C18 column as an enrichment column and detected by a diode array detector(DAD)to establish an online two-dimensional liquid chromatography analysis method.The pretreatment conditions of dansulfonyl chloride pre column derivatization method were optimized and methodological investigations on the established method from multiple aspects were conducted.Results The linear coefficient of taurine derivatives had good linearity in the range of 2.5-40.0μg/mL,and the correlation coefficient was greater than 0.999.The limit of detection was 1.2 mg/100 g,and the limit of quantitative was 4.0 mg/100 g,both of which were lower than the national standard method.The recoveries of taurine were 95.28%-97.58% and the relative standard deviations were 0.56%-1.38%,which could meet requirements for quantitation analysis of taurine in formula food for special medical purpose.Conclusion This method has a high degree of automation,short analysis time,high accuracy,and good repeatability,which is suitable for the determination of taurine in formula food for special medical use.
作者
李雨墨
迟秋池
顾正健
张庆临
陈燕
LI Yu-Mo;CHI Qiu-Chi;GU Zheng-Jian;ZHANG Qing-Lin;CHEN Yan(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)
出处
《食品安全质量检测学报》
CAS
2024年第18期298-305,共8页
Journal of Food Safety and Quality
关键词
牛磺酸
特殊医学用途配方食品
二维液相色谱法
taurine
formula food for special medical purpose
two-dimensional liquid chromatography
