Fritillaria flower extractive, preparation method therefore and applications
A technology of extract and fritillary flower, which is applied in the field of medicine, can solve the problems of complex ingredients, low content, and lack of versatility, and achieve the effect of simple operation and reasonable process
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Embodiment 1
[0031] Embodiment 1: peiminin A, peiminin B content assay method
[0032] Measured according to the "High Performance Liquid Chromatography Inspection Standard Operating Procedure" stipulated in the Pharmacopoeia.
[0033] Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; use acetonitrile as mobile phase A, 0.1% diethylamine as mobile phase B, carry out gradient elution as specified in the table below, evaporate light Scatter detector detection. The number of theoretical plates should not be less than 2000 based on the peak of peiminine A.
[0034] Table 1: Gradient elution conditions
[0035] time (min) Mobile phase A(%) Mobile phase B(%) 0-5 50 50 5-20 50-70 50-30 20-30 70-90 30-10
[0036] Preparation of reference substance solution: Take appropriate amounts of peiminin A reference substance and peiminin B reference substance, weigh them accurately, add methanol to make a mixed sol...
Embodiment 2
[0039] Example 2: Taking the content and transfer rate of peiminin A and peiminin B in the extract as an investigation index, the ethanol solution pH value, ethanol volume fraction, solid-liquid ratio, ultrasonic times, ultrasonic time, and relative density of thick paste and ethanol consumption.
[0040] 1. Take 10 g of Fritillaria flower powder, use 10 times the volume of 0.5% HCl, 0.05% HCl, 40% (v / v) ethanol solution of pH = 1, 2, 3, 4, 5, 6, ultrasonically extract 3 times , 1 hour each time, the filtrate was concentrated and dried, and the content of peiminin A + peiminin B in the extract and its transfer rate were determined.
[0041] The test results show that: when the pH is 3-4, the content and transfer rate of peiminin A + peiminin B in the extract are the best.
[0042] Table: 2: Influence of solvent acidity on extraction effect
[0043] 0.5% HCL 0.05% HCl pH=1 PH=2 pH=3 pH=4 pH=5 PH=6 content 0.326% 0.417% 0.469% 0.619% 1.694%...
Embodiment 3
[0070] Embodiment 3: purification process selection
[0071] Take the best extraction process to collect the filtrate and process it, then apply macroporous resin HPD100, HPD722, D101, neutral alumina column, Sephadex LH-20 dextran gel column, cation exchange resin column, collect effective parts, concentrate dry. Determination of the transfer rate and content of peimin A + peimin B.
[0072] The test results show that: Sephadex LH-20 Sephadex column has obvious advantages in transferring and enriching peimin A and peimin B.
[0073] Table 9: Comparison of extracts from different purification processes
[0074] Purification process HPD100 HPD722 D101 Neutral alumina LH-20 cation transfer rate 65.62% 60.31% 70.56% 58.69% 83.15% 75.49% content 16.67% 14.64% 19.78% 10.12% 46.59% 13.58%
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