在线净化二维液相色谱法测定特殊医学配方食品中的牛磺酸

Determination of taurine in food for special medical purpose by on-line purification two-dimensional high performance liquid chromatography

中文关键词:  牛磺酸  特殊医学用途配方食品  二维液相色谱

英文关键词:taurine  formula food for special medical purpose  two-dimensional liquid chromatography

中文摘要:

      目的 使用两泵一阀的二维液相色谱系统,建立特殊医学用途配方食品中牛磺酸在线净化二维液相色谱检测方法。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C18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,使样品能充分衍生并减少衍生所需时间。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 μg/mL~40.0 μg/mL范围内具有良好线性,相关系数r≥0.999；检出限为1.2 mg/100g,定量限为4 mg/100g；该方法回收率为95.28%~97.58%,相对标准偏差(relative standard deviation,RSD,n=6)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 本文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。

英文摘要:

      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 center cutting method was used to build an online two-dimensional liquid chromatography separation system. The C18 column was used as a one-dimensional column for preliminary separation and purification of sample solution, and the pentafluorophenyl(PFP) column was used as a two-dimensional column for secondary separation.The valve switching time was determined by the retention time of taurine derivatives on the one-dimensional chromatography, and the taurine derivatives were captured by the C18 column as an enrichment column. Investigated on the established method from multiple perspectives. Results The linear coefficient of taurine derivatives had good linearity in the range of 2.5 μg/mL~40.0 μg/mL，and the correlation coefficient(r) was greater than or equal to 0.999. The limit of detection was 1.2 mg/100g, and the limit of quantitative was 4 mg/100g, both of which were lower than the national standard method. The recovery of taurine was 95.28%-97.58% and the relative standard deviation （RSD, n=6） was 0.56%-1.38%, which could meet requirements for quantitative 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.