高效液相色谱法测定降糖型保健食品中的1-脱氧野尻霉素

Determination of 1-deoxynojirimycin in hypoglycemic health food by high performance liquid chromatography

中文关键词:  1-脱氧野尻霉素  柱前衍生  高效液相色谱法

英文关键词:1-deoxynojirimycin  precolumn derivatization  high performance liquid chromatography

中文摘要:

      目的 建立柱前衍生高效液相色谱法(high performance liquid chromatography, HPLC)测定保健食品中1-脱氧野尻霉素(1-deoxynojirimycin, 1-DNJ)的分析方法。方法 样品经水超声提取20 min, 在0.4 mol/L硼酸钾缓冲溶液(borate buffer solution, BBS)(pH=8.5)中, 1-DNJ与5 mmol/L芴甲氧羰酰氯(methoxycarbonyl chloride, FMOC-Cl)在20 ℃中水浴衍生30 min, 滤液采用HPLC进行检测。以乙腈+磷酸水溶液为流动相, 梯度洗脱。结果 1-DNJ 在1.0~20.0 μg/mL浓度范围内, 线性关系良好, 相关系数(r)=0.9993。回收率为90.96%~101.85%; 相对标准偏差(relative standard deviation, RSD)为1.9%~3.4%。结论 该方法前处理简便, 结果准确, 灵敏度较高, 适用于保健食品中1-DNJ含量测定。

英文摘要:

      Objective To establish a method for detection of 1-deoxynojirimycin (1-DNJ) in hypoglycemic health food by precolumn derivatization high performance liquid chromatography (HPLC). Methods The sample was ultrasonically extracted by water for 20 min. In 0.4 mol/L borate buffer solution (BBS) (pH=8.5), 1-DNJ and 5 mmol/L methoxycarbonyl chloride (FMOC-Cl) was heated in a water bath at 20 ℃ for 30 min and the filtrate was tested by HPLC. The gradient was eluted with acetonitrile+aqueous phosphoric acidas the mobile phase. Result 1-DNJ had good linearity in the concentration range of 1.0-20.0 μg/mL, and the correlation coefficient (r) was 0.9993. The recovery rate was 90.96%-101.85% and the relative standard deviation (RSD) was 1.9%-3.4%. Conclusion This method has the advantages of simple pretreatment, accurate result and high sensitivity, which is suitable for the determination of 1-DNJ content in health food.