Process for preparing high purity breviscapine B raw material medicine

[0020] Examples:

[0021] Weigh 1000g of commercially available scutellarin crude drug, add 5 times the volume of water, adjust the PH value to 7 with 20% disodium hydrogen phosphate test solution to completely dissolve, filter, add 8 times acetone to precipitate the filtrate, stir while adding, Make the precipitation complete, let stand for 10 hours, filter, add acetone and wash three times, then move the precipitate to another container, add 5 times the amount of 30% acetone, stir well, then add 20% hydrochloric acid to adjust the pH 1-2 static Let it stand for 10 hours, filter with suction, wash with water until it is neutral, wash with ethanol once, and dry to obtain refined scutellarin. The content of scutellarin by HPLC analysis is 99.43%, as shown in the figure.

[0022] Detection method: Chromatographic conditions and system suitability test (using octadecyl bonded silica as filler: methanol-0.1% phosphoric acid solution (40:60) as mobile phase; detection wavelength is 335nm. The number of theoretical plates is based on scutellarin The peak calculation should not be less than 5000). Take this product and dissolve it in 1ml of water for every 10mg of scutellarin, add methanol to make a solution containing about 0.4mg of scutellarin per 1ml, as the test solution; accurately measure 1.0ml of the test solution and place a 100ml measuring bottle In the middle, add methanol to the mark, mix well, as a control solution. Take 5ul of the control solution and inject it into the liquid chromatograph to adjust the detection sensitivity so that the peak height of the main component chromatographic peak is 10% of the full scale. Then take 5ul of the test solution and inject it into the liquid chromatograph, and record the chromatogram to 2.5 of the retention time of the main component peak. Measure the peak area of ​​each impurity on the chromatogram of the test solution and compare it with the peak area of ​​the main component of the control solution to calculate the purity of scutellarin.