The Fritillaria Total Alkaloid Preparation Technology And Quality Standards Research

Objective: To optimize extraction technology of total alkaloids from Fritillaria pallidiflorae bulbus and establish the quality control standards; Methods:1) the total alkaloid content and extract yield as response value was optimized by response surface methodology. 2) With adsorption capacity,specific solution desorption and total alkaloids as indexes, 12 different types of macroporous adsorption resin were selected by static and dynamic test. Sample solution concentration, the maximum loading amount, eluent type,eluent amount and other parameters were investigated 3) According to the 2010 edition of Pharmacopoeia, the characteristics of richment, thin layer identification, limit to check(moisture, ash content, heavy metals, extract) content have been studied. The sipeimine as index,use UV-VIS to determination total alkaloid content and use HPLC-ELSD determination the content of sipeimine. Results:1)Optimized extraction technology conditions was as following : 40 times of 70% ethanol, pH 2.0, extract 1 times, each time 1.5 h, the total alkaloid content reached11.04%,The total alkaloids of fritillaria extract rate reached 13.75%, 2)HPD-100(diameter/high=1:9)macroporous resin was selected as the best material in enrichment and purification of total alkaloids from Fritillaria pallidiflorae bulbus, the content of coumarin was 0.25 g·mL-1, pH value was 11,and with 70% ethanol, the volume was 9 BV, the flow rate was 1m L·min-1 According to the optimal purification process the content of total alkaloids was 70.50%, the yield was 43.0%. 3)Using home-made 2% NaOH silica thin layer plate,Chloroform-ethyl acetate-methanol- water(8:8.5:3.5:8.5) as developing solvent and with bismuth potassium iodide solution and sodium nitrite ethanol solution as colordeveloping agengt.Sipeimine was detected in the richment of bulbus Fritillaria pallidiflorae.the limit check all accord with pharmacopoeia standards. the total alkaloid content of the richment was 69.38%. The content of sipeimine was 0.24%. Conclusion:1)This modified extraction parameterswere credible and reliable with some practical value, Can be used for the extraction of total alkaloids from Fritillaria pallidiflorae bulbus. 2)The optimized technology is simple, stable,fit for separating and purifying ttotal alkaloids from Fritillaria pallidiflorae bulbus. 3) the quality control method of richment is accurate and feasible,can be used to effectively control the quality of richment of Bulbus Fritillaria pallidiflorae.