Study On The Chuanxiong Reference Extract Used In TLC

Chuanxiong comes from the plant Rhizome of Umbelliferae Ligusticum chuanxiong Hort.,which is a special medicine of Si chuan, widely used in pharmaceutical preparations. In the2010edition of "Chinese Pharmacopoeia",there are91prescription preparations were carried out with the Chuanxiong reference drug by the thin-layer indentification. In view of Chuanxiong reference drug containing volatile components, organic acids, such as poor stability ingredients, easy to be lost after crushing the chemical composition, is not conducive to the storage and use. Therefore, this study developed based on the reference medicinal materials research and technical requirements, and according to the requirements of "the Chinese pharmacopoeia2015edition concerning the research and preparation of reference extract which used in TLC". To study the extraction, purification, drying process, and equivalent homogeneity, and to prepare the chuanxiong reference extract used in TLC, which is easy to store and use, and carrying on the quality standard research, at the same time to study the stability of the finished product. The main research content and results are as follows:1. Study on the preparation of the Chuanxiong reference extractThe quality control of Chuanxiong We did quality inspection of Chuanxiong according to the2010edition Chinese Pharmacopoeia, and the medicine is qualified. We established the determination of ferulic acid and ligustilide in Chuanxiong by HPLC, the method is simple, accurate and reproducible.Extraction technology research Extracted by solvent method, with ferulic acid and ligustilide as an index, study on the extraction solvent, solvent dosage, extraction method, extraction time, extraction temperature, the single factor investigation for the single-factor, and using central composite design and response surface method to optimize the extraction process. The result is that using14times amount of73%ethanol, extracting2times, and per time is1.5hours, the extract temperature was83℃. Purification technology research Extract were purified by macroporous adsorption resin, with ferulic acid and ligustilide adsorption rate and the resolution of this lactone as an index.examined the adsorption capability to study the elution process of macroporous resin. The result indicates that optimum purification process is as follows:HPD-100macroporous resin, diameter ratio1:10, drug liquid concentraton0.2g/mL,5BV, with2BV distilled water,3BV10%ethanol,4BV20%ethanol,3BV30%ethanol,5BV50%ethanol,4BV60%ethanol in turn, collect and merge20%ethanol,30%ethanol,50%ethanol and60%ethanol elution part, ferulic acid elution rate and ligustilide elution rate were both higher than80%, purified yield about4.9%.Drying technology research Recovered of ethanol from eluent and concentrated under reduced pressure to a certain volume, precooled extracts for12hours to make fully freezing at-20℃, and then placed it in a vacuum freeze-drying apparatus and dried for6hours, crushed into fine powder.Equivalent homogeneity According to the standard of the dosage and extraction of reference drug, converted and compared the dosage of the medicine equivalent to extract, to ensure the consistency of the amount.2. Study on the quality standard of Chuanxiong reference extractStudy on the charaters of Chuanxiong reference extract of quality control, including solubility, identification, examination and content determination and stability. Chuanxiong reference extract solubles in methanol, ethanol, slightly solubles in ethyl acetate, ethyl ether, slightly soluble in water. TLC was established to identify extract. Checked the moisture and total ash content. Established the determination of ferulic acid and ligustilide in Chuanxiong by HPLC, and3batches of samples were determined, each batch content is basically stable. Tentatively ferulic acid content is stipulated not less than7.5%, ligustilide content not less than11.5%. Stability factor investigation and accelerated stability test has carried on, and the results show that the reference extract should be shading, sealing, and stored at low temperature set.