| Objective: Study had been carried from the foundation of content Iimitation for medicalmaterial, extraction and macroporous resin purification of active ingredient HE-Ⅲfrom Nigella glandulifera Freyn et Sint, foundation of content Iimitation forintermediate. The aim is to develop a new drug, which has the character of definiteeffective fraction, enrichment of the active components, well-controlled in quality andused convenient．Methods: HE-Ⅲ was the main constituent in Nigella glandulifera Freyn et Sint，whichwas used as the reference substance to establish HPLC method for the determination ofthe content of HE-Ⅲ, and initially set content limit. The yield of HE-Ⅲ was used toevaluate the extraction technology through single factor experiment and uniformexperiment design. Using the yield and content of HE-Ⅲas the evaluation standard,suitable macreporous resin was chosen by static adsorption and desorption test. Othertechnology parameters were optimized by orthogonal experiment design. The content ofHE-Ⅲ was chosen to estimate the quality control of the intermediate and the contentlimitation was established at the sarne time．Results: Preliminary determination of not less than2.00%HE-Ⅲ in medicinal material.The optimal condition of the extracting HE-Ⅲ was10-fold70%ethanol, extracted3times,1h per time. The yield and extraction rate were2.56%and93.09%in theoptimized extraction process. The optimized purification process were summarized asfollows: AB-8macroporous resin, ratio of diameter to height of resin column1:3,sample concentration0.25g·ml-1, feed rate1.5BV·h-1, eluted with7BV of distilled water and6BV of70%ethanol, elution velocity3BV·h-1, the70%ethanol eluent wascollected, the yield of HE-Ⅲ was76.36%and the purity was53.53%. The content ofHE-Ⅲ in the intermediate of not less than45.0%.Conclusion: Optimized process was simple, stable with good repeatability, which wassuitable for industrial production. |
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