Identification of ox bile powder

Moisture must not exceed 5.0% "Chinese Pharmacopoeia" 2010 Edition Appendix Ⅸ H Method 1

Take 0.1g of this product, add 10ml of methanol, dissolve it by superbirth treatment, filter, and steam the filtrate on a water bath until nearly dry, dissolve it in 5ml portions with 2.5mol/L sodium hydroxide solution, and transfer it to a test tube with a stopper After being hydrolyzed on the water bath for 5 hours, take it out, let it cool, add hydrochloric acid dropwise to adjust the PH value to 2~3, extract 3 times with ethyl acetate, 10ml each time. The combined ethyl acetate solution was shrunk to dryness, and the residue was dissolved by adding 1 ml of methanol as the test solution. Take another hyodeoxycholic acid reference substance, add methanol to make a solution containing 1mg per 1ml, as the reference substance solution. According to the test of thin layer chromatography (Appendix VI B), draw 2μL of each of the above two solutions and place them on the same silica gel G thin-layer plate, using isooctane-n-butanol-glacial acetic acid (8:5:5) as Expand the developing agent, take it out, dry it, and heat it with 10% phosphomolybdic acid ethanol solution at 105°C until the spots appear clear. In the chromatogram of the test product, no spots of the same color shall be displayed in the position corresponding to the control chromatogram.

Preparation of reference substance solution Take 12.5mg of cholic acid reference substance, accurately weigh it, place it in a 25ml measuring flask, add 60% glacial acetic acid solution to dissolve it, dilute to the mark, and shake well to obtain (each 1ml contains cholic acid 0.5 mg)