摘要
目的：运用筛选实验设计联合星点设计效应面法，优化干姜提取工艺；方法：以姜酮、6一姜辣素的含量为指标，浸泡时间，液固比，溶剂DH值，提取时间，提取次数，提取温度及浓缩温度为考察因素，采取PB-CCD优选提取工艺条件。采用Agilent 5TC-C18（2）色谱柱（250mm×4．6mm，5μm）；流动相A相为（0．1％甲酸-水），B相为乙腈，梯度洗脱；流速为1．0mL·min-1，检测波长为254nm和280nm，对姜酮、6-姜辣素进行含量测定方法研究。结果：干姜最佳水提工艺为浸泡时间：1h，提取时间3h，液固比：12，pH值为9．0，提取温度：70℃，提取次数：4次，浓缩温度：88℃。姜酮线性范围为3～25g·mL-1，r=O．999，平均回收率为103．71％，RSD％为0．80％（n=3）；6-姜辣素，线性范围为15-125g·mL-1，r=0．999，平均回收率为100．67％，RSD％为1．45％（n=3）。结论：本实验确定了干姜提取的主要影响因素及工艺参数，建立了姜酮、6-姜辣素含量测定方法。
Objective： Using Plackett-burman design combined with central composite design （CCD） response surface methodology, to examine the significance of influence factors. Methods： Taking the content of Zingerone and 6-gingerol as indexes, with Soak time, liquid-solid ratio, solvent, pH value, extraction time, extraction times, extraction temperature and concentration temperature as examine factors, using the PB-CCD to optimize water extraction process conditions and determine content. The chromatographic conditions： Agilent 5 TC-Cls（2）chro- matographic column（250 mm×4.6 mm, 5 μm）; Mobile phase for A phase （0.1% formic acid and water）, B phase for acetonitrile, gradient elution; flow rate 1.0 mL ·min-1, three-way splitter; Column temperature 30 ℃; sample size 10 μL, taking 254 nm and 280 nm as detection wavelength. Results： The best water extraction process for extracting time 3 h, Liquid-solid ratio： 12.0, pH 9, immersion time：l.1 h, extract temperature： 70 ℃, extraction times： g times, concentration temperature： 88℃. Linear range of zingerone was 3-25 g· mL-1, r=0.999, the average recovery rate was 103.71%, RSD%=0.8% （n=3）, Linear range of 6-gingerol was 15～125 g·mL-1, r=0.999, the av- erage recovery rate was 100.67%, RSD%=1.45% （n=3）. Conclusion： This experiment determined the optimal tech- nology of Rhizoma zingiberis water extraction and content determination.
出处
《中医药导报》
2016年第18期53-56,共4页
Guiding Journal of Traditional Chinese Medicine and Pharmacy
基金
陕西省科技统筹创新工程计划项目(2011KTCG03-02)
陕西省重点科技创新团队计划项目(2012KTC-20)
