摘要
目的:采用星点设计-效应面法优选优选石斛的酒润蒸制工艺。方法:采用HPLC测定石斛碱含量,色谱条件为Diamonsil钻石二代C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-水(0.1%三乙胺)梯度洗脱(0～30 min,30%～80%乙腈;30～40 min,80%乙腈),流速1 mL·min-1,检测波长240 nm,柱温30℃,进样量10μL。利用UV测定石斛多糖含量,以白酒体积分数、白酒加入量、蒸制时间为自变量,石斛碱与石斛多糖含量的总评归一值为因变量,通过星点设计-效应面法优选石斛的炮制工艺。结果:石斛碱线性范围0.336～3.36μg(R2=0.999 8),精密度RSD 1.24%,重复性RSD 1.06%,平均加样回收率97.62%(RSD 1.45%);石斛多糖线性范围0.020 32～0.101 6 g·L-1(R2=0.997 1),精密度RSD 1.71%,重复性RSD1.90%。最佳炮制工艺为白酒体积分数48%,白酒加入量17%,蒸制时间6.78 h。石斛碱平均质量分数0.303%,预测值0.292%,相对偏差3.76%;多糖平均质量分数12.3%,预测值11.8%,相对偏差4.24%,建立的模型预测性良好。结论:优选的石斛酒润蒸制工艺简便、稳定。
Objective： To optimize streamed processing technology of Dendrobii Caulis with wine by central composite design-response surface methodology. Method： The content of dendrobine was determined by HPLC, chromatographic conditions were as follows： Diamonsil C18 column （4.6 mm - 250 mm, 5 μm） , mobile phase of acetonitrile-water （0. 1% triethylamine） gradient elution, flow rate 1 mL ·min-1, detection wavelength 240 nm, column temperature 30 ℃ , injection volume 10 μL. The content of polysaccharides was determined by UV. With the concentration and amount of wine, steaming time as independent variables, overall normalized value of the contents of dendrobine and polysaccharides as dependent variable, processing technology was optimized by central composite design-response Surface methodology. Result： Linear range of dendrobine was 0. 336-3.36 μg （R2 = 0. 999 8）, RSD of precision was 1.24% , RSD of repeatability was 1.06% , average recovery was 97.62% （RSD 1.45% ） ; Linear range of polysaccharides was 0. 020 32-0. 101 6 g ·L^-1 （R2 = 0. 997 1 ） , RSD of precision was 1.71% , RSD of repeatability was 1.90%. Optimum processing conditions were ： the concentration of wine 48% , the amount of wine 17% and steaming time 6.78 h. Deviation between the predicted value （0. 292% ） and the measured value （0. 303% ） of the mass fraction of dendrobine was 3.76% , while deviation between the predicted value （11.8%） and the measured value （12.3%） of polysaccharides was d. 24% , established model had a good prediction. Conclusion： Optimized processing technology was simple and stable.
出处
《中国实验方剂学杂志》
CAS
北大核心
2013年第19期34-37,共4页
Chinese Journal of Experimental Traditional Medical Formulae
基金
重庆市卫生局中医药科技项目(2011-2-168)
关键词
金钗石斛
石斛碱
石斛多糖
炮制工艺
高效液相色谱法
星点设计-效应面法
Dendrobii Caulis
dendrobine
polysaccharides from Dendrobii Caulis
processingtechnology
HPLC
central composite design-response surface methodology
