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作 者:毕艳艳 郝大伟 代立平 唐伟铭 龙瑞 沈庆国 BI Yan-yan;HAO Da-wei;DAI Li-ping;TANG Wei-ming;LONG Rui;SHEN Qing-guo(Lunan Houpu Pharmaceutical Co.,Ltd.,Linyi 276006,China;State Key Laboratory of Generic Manufacture Technology of Traditional Chinese Medicine,Linyi 276006,China)
机构地区:[1]鲁南厚普制药有限公司,山东临沂276006 [2]中药制药共性技术国家重点实验室,山东临沂276006
出 处:《中国现代中药》2022年第2期314-319,共6页Modern Chinese Medicine
基 金:国家重点研发计划项目(2019YFC1711200);临沂市兰山区科技创新发展计划专项(1942)。
摘 要:目的:优化硅胶柱色谱纯化胡黄连苷Ⅱ最佳工艺条件。方法:以洗脱剂三氯甲烷-甲醇的比例、色谱硅胶-上样样品(原药材)质量比、洗脱流速为考察因素,以胡黄连苷Ⅱ质量分数、回收率为考察指标。在单因素试验的基础上,运用响应面法进行优化,确定硅胶柱色谱纯化胡黄连苷Ⅱ最佳工艺条件,并进行3批验证实验。结果:最佳纯化工艺条件为洗脱剂三氯甲烷-甲醇6∶1,色谱硅胶-上样样品(原药材)质量比1.7∶1.0,洗脱流速7 mL·min^(-1),胡黄连苷Ⅱ质量分数可达到54.99%,回收率为93.59%。结论:响应面法确定的工艺简单可行,可用于硅胶柱色谱纯化胡黄连苷Ⅱ。Objective:To optimize the purification of pricrosideⅡ by column chromatography on silica gel.Methods:Based on the single factor experiments,the response surface methodology was used to optimize the purification of pricroside Ⅱ by column chromatography on silica gel with chloroform/methanol ratio,the mass ratio of silica gel/the loading sample(original medicinal material),and the elution flow rate as the factors,and the mass fraction and the recovery rate of pricroside Ⅱ as the indicators.Verification experiments were carried out in triplicates.Results:The mass fraction and recovery rate of pricroside Ⅱ reached 54.99% and 93.59%,respectively under the optimal purification parameters,i.e.,chloroform/methanol ratio of 6∶1,silica gel/the loading sample(original medicinal material) mass ratio of 1.7∶1.0,and the elution flow rate of 7 mL·min^(-1).Conclusion:The process optimized by response surface methodology is convenient and feasible,and it can be used for the purification of pricroside Ⅱ by column chromatography on silica gel.
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