Content determination:
Emodin was determined according to HPLC determination.
Chromatographic conditions and system suitability test:
Use ODS as filler，methanol-0.1% phosphoric acid solution (80:20) as mobile phase; detection wavelength as 254nm. The number of theoretical plates should not be less than 3000 according to emodin peak.
Preparation of reference substance solution:
Take an appropriate amount of emodin reference substance that has been dried under reduced pressure with phosphorus pentoxide as a desiccant for 24 hours, accurately weighed, and add methanol to make a solution containing 48ug per lml, then get it.
Preparation of the test solution:
Take the powder (passed through No. 3 sieve) about 0.1g, accurately weigh it, add 25ml of chloroform and 20ml of 2.5mol/L sulfuric acid solution, weigh it, and place it at 80° Heat to reflux in a water bath for 2 hours, cool to room temperature, and then weigh it. Use chloroform to make up the lost weight and shake it well. Dilute the chloroform solution, accurately measure 10ml, evaporate to dryness, add methanol to the residue to dissolve, transfer to a 10ml volumetric flask, add methanol to dilute to the mark, shake well, filter, take the additional filtrate, then get it.
Determination method:
Accurately draw 5ul each of the reference solution and the test solution, inject it into HPLC instrument for determination.
Calculated as a dried product, contains emodin (C15H10O5) not less than 0.60%.
Polygonatum:
Avoid light operation. According to HPLC determination.
Chromatographic conditions and system suitability test:
Use ODS as filler; acetonitrile-water (23:77) as mobile phase; detection wavelength as 306nm. The number of theoretical plates should not be less than 3000 based on the peak of polydatin.
Preparation of reference substance solution:
Take an appropriate amount of polydatin reference substance that has been dried under reduced pressure with phosphorus pentoxide as a desiccant for 24 hours, accurately weighed, and add dilute ethanol to make a solution containing 15ug per lml, then get it.
Preparation of the test solution:
Take about 0.1g of the powder (passed through No. 3 sieve), accurately weigh it, add 25ml of dilute ethanol, weigh it, heat to reflux for 30 minutes, cool to room temperature, and then weigh it. Dilute ethanol to make up the lost weight, shake well, take the supernatant, filter, and take the filtrate then get it.
Determination method:
Accurately draw 10ul each of the reference solution and the test solution, inject it into HPLC instrument for determination,then get it.
Calculated as a dried product and contains not less than 0.15% of polydatin (C20H22O8).