Page 103 - 2019年9月第30卷第18期

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 Δ

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王仁广 ，杨净尧 ，张欣舒 ，邱智东 ，陈 新 ，贾艾玲 （1.长春中医药大学药学院中药有效成分省部共建教
育部重点实验室，长春 130117；2.成都中医药大学药学院，成都 611137）
中图分类号 R284.2 文献标志码 A 文章编号 1001-0408（2019）18-2546-06
DOI 10.6039/j.issn.1001-0408.2019.18.18
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。
关键词 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

Optimization of Water Extraction Technology of Saikosaponin a and Saikosaponin d from Bupleurum
chinense by Electromagnetic Cracking
WANG Renguang ，YANG Jingyao ，ZHANG Xinshu ，QIU Zhidong ，CHEN Xin ，JIA Ailing 1， 2 （1. Key
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Laboratory of TCM Active Ingredient of Ministry of Education，School of Pharmacy，Changchun University of
TCM，Changchun 130117，China；2. College of Pharmacy，Chengdu University of TCM，Chengdu 611137，
China）
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 μ g/mL，respectively. The detection limits were 0.05 and 0.04 μ g/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.
Δ 基金项目：吉林省科技发展计划项目（No.20160201001YY、
KEYWORDS Bupleurum chinense；Saikosaponin a；Saiko-
20170623055TC）；长春中医药大学百名中青年骨干教师培养计划
saponin d；HPLC；Box-Behnken response surface methodo-
＊ 博 士 研 究 生 。 研 究 方 向 ：中 药 制 剂 新 技 术 。 电 话 ：0431-
86172786。E-mail：727736000@qq.com logy；Water extraction technology；Content determination；
# 通信作者：讲师，博士研究生。研究方向：中药制剂。电话： Electromagnetic cracking
0431-86172786。E-mail：171265932@qq.com

·2546 · China Pharmacy 2019 Vol. 30 No. 18 中国药房 2019年第30卷第18期