摘要
建立水浴震荡提取-高效液相色谱法测定黑米中矢车菊素-3-葡萄糖苷(Cy-3-G)的方法。确定了HPLC法测定Cy-3-G的测定条件,通过响应面优化试验确定了水浴震荡提取黑米中Cy-3-G的最优提取条件。实验得HPLC法测定Cy-3-G的条件为:色谱柱(C18,150mm×4.6mm,5um),柱温30℃,进样体积10u L,检测波长520nm,流动相A(甲醇)-B(1%甲酸水溶液),流速1m L/min,梯度洗脱:0~3min,A∶B(20∶80);3~17min,A∶B(20∶80~30∶70);17~20min,A∶B(30∶70~20∶80)。最优提取条件为:溶剂是含0.8%盐酸的50%乙醇水溶液、料液比1∶20、提取次数2次、温度70℃、时间20min,Cy-3-G的得率为0.728%。结果表明水浴震荡提取法实现了黑米中Cy-3-G的高效提取,满足样品测定的前处理需求;建立的HPLC法测定黑米中Cy-3-G的方法操作简便、重复性好、测定结果精密度高。
To establish HPLC detection method of cyanidin-3-glucoside in Black rice extracted by water bath shaking method. The best detection conditions were determined. The optimum extraction conditions of Cy-3-G extracted by water bath shaking extraction were obtained through response surface design. The HPLC detection conditions of Cy-3-G were： chromatographic column （C18, 150mm × 4.6mm, 5um）, the column temperature was 30℃, the injection volume was 10uL, the detection wavelength was 520nm, mobile phase of A （methanol） -B （ 1% formic acid）, the flow rate was lml.Jmin, gradient elution was as follow ： 0 - 3min, A ： B （20 ： 80）, 3 - 17min, A ： B （20 ： 80 - 30 ： 70）, 17 - 20rain, A ： B （30 ： 70 - 20 ： 80）. The optimum extraction conditions were as follows： solvent of 50% ethanol aqueous solution containing 0.8% hydrochloric acid, the solid-liquid ratio was 1 ： 20, extracted two times, extraction temperature was 70 ~C, extraction time was 20min. The extraction yield of Cy-3-G was 0.728%. The results showed that the water bath shaking extraction method achieved effective extraction of Cy-3-G in Black rice, and satisfied the requirement of sample preparation. The HPLC detection method of Cy-3-G in Black rice showed the advantages of simple operation, good repeatability and determination results with high precision.
作者
刘长姣
熊湘炜
郑霞
杨柳
陈宇飞
LIU Chang-jiao XIONG Xiang-wei ZHENG Xia YANG Liu CHEN Yu-fei(Jilin Province Key Laboratory of Grain and Oil Processing of Jilin Business and Technology College, Changchun 130507)
出处
《中国食品添加剂》
北大核心
2017年第9期210-215,共6页
China Food Additives
基金
吉林省教育厅"十二五"科学技术研究项目(2014439)
