Box-Behnken响应面法优化管花肉苁蓉中毛蕊花糖苷的提取工艺研究
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篇名: Box-Behnken响应面法优化管花肉苁蓉中毛蕊花糖苷的提取工艺研究
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摘要: 目的:优化管花肉苁蓉中毛蕊花糖苷的提取工艺,为该药材的深入开发和综合利用提供参考。方法:采用高效液相色谱法对管花肉苁蓉中的毛蕊花糖苷进行含量测定。色谱柱为Inertsil-ODS-3V,流动相为甲醇-0.2%甲酸水溶液(40 ∶ 60,V/V),流速为1 mL/min,柱温为30 ℃,检测波长为330 nm,进样量为10 μL。以毛蕊花糖苷的提取率为考察指标,分别对浸泡时间、乙醇浓度、液料比、提取时间、提取次数进行单因素试验;根据上述试验结果采用Box-Behnken响应面法对乙醇浓度、液料比、提取时间等条件进行优化,并对优化后的提取工艺进行验证试验。结果:毛蕊花糖苷检测质量浓度的线性范围为18.65~932.4 μg/mL。最优提取工艺为乙醇浓度63%、液料比8 ∶ 1(mL/g)、浸泡2 h、提取时间1.5 h、提取2次。3次平行验证试验所得毛蕊花糖苷的提取率分别为78.21%、76.95%、79.34%,与预测值76.76%的相对误差分别为1.89%、0.25%、3.36%。结论:优化所得管花肉苁蓉中毛蕊花糖苷的提取工艺稳定、可行,适用于该化合物的提取。
ABSTRACT: OBJECTIVE: To optimize the extraction technology of verbascoside from Cistanche tubulosa, and to provide reference for further development and comprehensive utilization of C. tubulosa. METHODS: The content of verbascoside in C. tubulosa was determined by HPLC. The determination was performed on  Inertsil-ODS-3V  column with  mobile phase consisted of methanol-0.2% formic acid aqueous solution (40 ∶ 60, V/V) at  the flow rate  of  1 mL/min. The column temperature was 30 ℃, the detection wavelength was 330 nm, and the sample size  was 10 μL. Using extraction rate of verbascoside as index, soaking time, ethanol concentration, liquid-solid ratio, extraction time and extraction times were investigated by single factor tests. According to the results of above tests, ethanol concentration, liquid-solid ratio and extraction time were optimized by Box-Behnken response surface methodology. The verification tests were carried out on the optimized extraction technology. RESULTS: The linear range of verbascoside was 18.65-932.4 μg/mL. The optimal extraction technology included that ethanol concentration 63%, liquid-solid ratio 8 ∶ 1 (mL/g), soaking for 2 h, extraction time 1.5 h, extracting for 2 times. The extraction rates of verbascoside in the three parallel verification tests were 78.21%, 76.95%, 79.34%, respectively. The relative errors of those to predicted value 76.76% were 1.89%, 0.25%, 3.36%. CONCLUSIONS: The optimized extraction technology of verbascoside from C. tubulosa is stable and feasible, and is suitable for the extraction of verbascoside.
期刊: 2019年第30卷第14期
作者: 孔征,毛乐静,霍仕霞,苏娅,姜萌,闫明
AUTHORS: KONG Zheng,MAO Lejing,HUO Shixia,SU Ya,JIANG Meng,YAN Ming
关键字: 管花肉苁蓉;毛蕊花糖苷;响应面法; Box-Behnken 设计;提取工艺;优化
KEYWORDS: Cistanche tubulosa; Verbascoside; Response surface methodology; Box-Behnken design; Extraction technology; Optimization
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