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柴胡中柴胡皂苷a、柴胡皂苷d的电磁裂解水提取工艺优化
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| 篇名： | 柴胡中柴胡皂苷a、柴胡皂苷d的电磁裂解水提取工艺优化 |
| TITLE： | |
| 摘要： | 目的：建立同时测定柴胡水提液中柴胡皂苷a、柴胡皂苷d含量的方法，并优化其电磁裂解水提取工艺。方法：采用高效液相色谱法。色谱柱为SB-C18，流动相为乙腈-水（梯度洗脱），柱温为40 ℃，流速为1.0 mL/min，检测波长为210 nm，进样量为10 μL。在单因素试验基础上，以提取时间、物料粒度、料液比为考察因素，柴胡皂苷a与柴胡皂苷d的总提取率为响应值，采用Box-Behnken响应面法优化其提取工艺，并与超声法和煎煮法进行比较。结果：柴胡皂苷a、柴胡皂苷d检测质量浓度的线性范围分别为50.70～202.80 μg/mL（r＝0.999 9）、50.50～202.00 μg/mL（r＝0.999 9）；定量限分别为0.16、0.13 μg/mL，检测限分别为0.05、0.04 μg/mL；精密度、稳定性、重复性的RSD均小于2％；加样回收率分别为98.23％～102.47％（RSD＝1.80％，n＝6）、98.84％～102.06％（RSD＝1.60％，n＝6）。最优提取工艺为以水提取1次，提取时间2.50 min、药材过80目筛、料液比1 ∶ 28（g/mL）。3次验证试验结果显示，最优工艺所得柴胡皂苷a与柴胡皂苷d的平均总提取率为8.42 mg/g，高于超声法（8.34 mg/g）和煎煮法（8.06 mg/g），且提取时间更短。结论：所建含量测定方法简便、准确，可用于同时测定柴胡水提液中柴胡皂苷a、柴胡皂苷d的含量；优化所得电磁裂解水提取的工艺稳定、可行。 |
| ABSTRACT： | OBJECTIVE： To establish the method for simultaneous determination of saikosaponin a and saikosaponin d in Bupleurum chinense water extract， and to optimize its water extraction technology for electromagnetic cracking. METHODS： HPLC method was used. The determination was performed on SB-C18 column with mobile phase consisted of acetonitrile-water （gradient elution） at the flow rate of 1.0 mL/min. The column temperature was 40 ℃. The detection wavelength was set at 210 nm， and the sample size was 10 μL. Based on single factor experiment， using extraction time， particle size， solide-liquid ratio as factors， total extraction rate of saikosaponin a to saikosaponin d as indexes， the extraction technology was optimized by using Box-Behnken response surface methdology， and compared with the results of ultrasound method and decoction method. RESULTS： The linear range of saikosaponin a and saikosaponin d were 50.70-202.80 μg/mL （r＝0.999 9） and 50.50-202.00 μg/mL （r＝0.999 9）， respectively. The quantitation limits were 0.16 and 0.13 μg/mL， respectively. The detection limits were 0.05 and 0.04 μg/mL，respectively. RSDs of precision， stability and reproducibility tests were all lower than 2％. The average recoveries were 98.23-102.47％ （RSD＝1.80％， n＝6） and 98.84％-102.06％ （RSD＝1.60％， n＝6）. The optimal extraction technology was as follows： the extraction time of 2.50 min； the particle size of 80 mesh， solid-liquid ratio of 1 ∶ 28 （g/mL）. Results of 3 times of validation tests showed that the optimal technology included the average total extraction rates of saikosaponin a and saikosaponin d were 8.42 mg/g， which was higher than that of ultrasonic method （8.34 mg/g） and decoction method （8.06 mg/g）， and the extration time was shorter. CONCLUSIONS： Established method is simple and accurate， and can be used for simultaneous determination of saikosaponin a and saikosaponin d in B. chinense water extract. The optimized water extraction technology for electromagnetic cracking is stable and feasible. |
| 期刊： | 2019年第30卷第18期 |
| 作者： | 王仁广，杨净尧，张欣舒，邱智东，陈新，贾艾玲 |
| AUTHORS： | WANG Renguang，YANG Jingyao，ZHANG Xinshu，QIU Zhidong，CHEN Xin，JIA Ailing |
| 关键字： | 柴胡；柴胡皂苷a；柴胡皂苷d；高效液相色谱法；Box-Behnken响应面法；水提取工艺；含量测定；电磁裂解 |
| KEYWORDS： | Bupleurum chinense； Saikosaponin a； Saiko- saponin d； HPLC； Box-Behnken response surface methodo- logy； Water extraction technology； Content determination； Electromagnetic cracking |
| 阅读数： | 616 次 |
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