摘要
目的优化龙胆标准提取物的制备工艺，建立龙胆标准提取物中龙胆苦苷的含量测定方法。方法采用L9（3^4）正交实验设计优化龙胆的提取工艺和XDA-1大孔树脂纯化条件；建立高效液相色谱测定标准提取物中龙胆苦苷含量的方法。结果龙胆最佳提取条件为：药材最粗粉加10倍量水，回流提取3次，每次1h，水提浸膏中龙胆苦苷含量、以龙胆苦苷计提取率及浸膏得率分别为4．40％、100．4％和57．49％。大孔树脂纯化条件为上样液中龙胆苦苷浓度8．0g·L^-1，pH4，上样液流速0．13mL·min^-1，大孔树脂XDA-1对龙胆苦苷的吸附量达到62．26mg·g^-1；以31．50mL的水和94．50mL的20％乙醇梯度洗脱，流速分别为0．50，0．25mL·min^-1，制得的龙胆标准提取物中龙胆苦苷含量为32．20％，是水提浸膏含量的7倍，从药材到标准提取物的转移率以龙胆苦苷计为79．2％。龙胆苦苷浓度在0．22～13．84g·L^-1内与色谱峰面积呈良好的线性关系（r=0．9995），平均加样回收率为96．88％，RSD为1．10％。结论水煎法结合大孔树脂富集是制备龙胆标准提取物的有效方法。高效液相色谱法可用于龙胆标准提取物中龙胆苦苷的质量控制，为更深入的研究龙胆标准提取物提供了基础。
OBJECTIVE To optimize preparation process of standard extract from Radix Gentianae and establish a quality standard for the standard extract. METHODS L9 （ 3^4 ） orthogonal experiment was used to optimize the extraction process of Radix Gentianae and the adsorption conditions on XDA - 1 macroporous resin. HPLC was used for determining the content of gentiopicroside in the standard extract. RESULTS The optimal conditions for extraction were as follows：most coarse powder of Radix Gentianae was extracted with 10 times water for 1 h, for three times. The contents of gentiopicroside in the extract, extractability and extraction yield were 4.40% , 100.4% and 57.49%. The optimal parameters for adsorption were ： concentration of feed solution 8.0 g · L^-1, pH 4, flow rate 0. 13 mL · min ^-1. The adsorption capacity was determined as 62. 26 mg · g^-1 on XDA - 1 resin. The gradient elution program was：water for 31.50 mL, flow rate 0. 5 mL · min^-1 ; then 20% ethanol for 94. 50 mL, flow rate 0. 25 mL · min^-1. After one run treatment with XDA - 1 resin, the concentration of gentiopicroside in the product was increased from 4.4% to 32.20% as 7.0-fold as the untreated extract. The recovery yield was 79. 2% from Radix Gentianae. The content of gentiopicroside showed a good linearity with the area of peak in the range of 13.84 - 0. 22 g · L^-1 （ r = 0. 999 5 ）, the average recovery rate was 96. 88% and RSD was 1.10%. CONCLUSION Extraction with water and enrichment with macroporous resin were effective methods for preparation of standard extract from Radix Gentianae. HPLC method can be used for quality control of the standard extract. The study was beneficial for the further research of standard extract from Radix Gentianae.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2008年第24期1909-1913,共5页
Chinese Pharmaceutical Journal
基金
上海市科学技术委员会科研项目资助课题(04DZ19851)
上海市重点学科建设资助项目(Y0301)资助
关键词
龙胆标准提取物
龙胆苦苷
正交设计
大孔树脂
含量测定
standard extract from Radix Gentianae
gentiopicroside
orthogonal design
macroporous resin
quantitative determination
作者简介
鲁艳柳，女，博士研究生。
通讯作者：王长虹，男，博士，研究员Tel：（021）51322513,Fax：（021）51322519.E—mail：wchcxm@163．com
