独一味总环烯醚萜苷分离纯化工艺的优化
目的:优化独一味总环烯醚萜苷的制备工艺,获取纯度相对较高的总环烯醚萜苷。方法以甲醇唱水为流动相,梯度洗脱方式建立分离分析独一味总环烯醚萜苷的高效液相色谱方法,实现各组分的最佳分离,统计、记录其三维吸收图谱,并结合紫外全波长扫描,对前期制备的独一味总环烯醚萜苷中影响纯度的杂质特征进行分析,根据杂质特性优化大孔树脂结合聚酰胺柱制备过程,紫外实时监测,剔除杂质,产品溶液经冷冻干燥获得冻干粉,并以 HPLC对比前后制备工艺产品成分差异。结果工艺优化前产品中环烯醚萜苷含量为69.06%,优化后含量为90.60%,含量提升21.54%;本次制备总产率为16.70%(以水提取物的质量为参照),总环烯醚萜苷转...
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| Published in | 药学实践杂志 Vol. 34; no. 5; pp. 416 - 420 |
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| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
银川市妇幼保健院药剂科,宁夏银川750001%银川市妇幼保健院药剂科,宁夏银川,750001%兰州军区兰州总医院药剂科/全军高原特殊环境损伤防治重点实验室,甘肃 兰州,730050
2016
兰州军区兰州总医院药剂科/全军高原特殊环境损伤防治重点实验室,甘肃 兰州730050 |
| Subjects | |
| Online Access | Get full text |
| ISSN | 1006-0111 |
| DOI | 10.3969/j.issn.1006-0111.2016.05.009 |
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| Summary: | 目的:优化独一味总环烯醚萜苷的制备工艺,获取纯度相对较高的总环烯醚萜苷。方法以甲醇唱水为流动相,梯度洗脱方式建立分离分析独一味总环烯醚萜苷的高效液相色谱方法,实现各组分的最佳分离,统计、记录其三维吸收图谱,并结合紫外全波长扫描,对前期制备的独一味总环烯醚萜苷中影响纯度的杂质特征进行分析,根据杂质特性优化大孔树脂结合聚酰胺柱制备过程,紫外实时监测,剔除杂质,产品溶液经冷冻干燥获得冻干粉,并以 HPLC对比前后制备工艺产品成分差异。结果工艺优化前产品中环烯醚萜苷含量为69.06%,优化后含量为90.60%,含量提升21.54%;本次制备总产率为16.70%(以水提取物的质量为参照),总环烯醚萜苷转移率为74.72%(相对于水提取物中总环烯醚萜苷的质量)。结论优化过程简单,操作步骤可控,易于实现,纯化效果显著。 |
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| Bibliography: | 31-1685/R TAO Rui1,2, FU Meng2, CAO Xinyuan1, LI Maoxing1 (1. Department of Pharmacy, Lanzhou General Hospital of PLA, Key Laboratory of the Prevention and Cure for the Plateau Environment Damage, PLA, Lanzhou 730050, China; 2. Pharmacy of Yinchuan Maternal and Child Health Care Hospital, Yinchuan 750001, China) Lamiophlomisrotata (Benth.) ; iridoids glycosides; preparation; process optimization; content Objective To obtain iri doid glycosides with relatively high purity by the optimization of the preparation process of iridoid glycosides from Lamioplomisrotata .Methods Used methanol-water mobile phase with gradient run to set up an HPLC method and achieved the best separation of each composition .Recorded and calculated statistics for its three-dimen-sional absorption spectrum combined with UV visible wavelength scanning to analyze the characteristics of the impurities , which have affected the purity of previous preparations of iridoid glycosides from Lamioplomisrotata .To optimize the process , a macroporous |
| ISSN: | 1006-0111 |
| DOI: | 10.3969/j.issn.1006-0111.2016.05.009 |