Polygonum perfoliatum medicinal material, method for preparing reference substance of active constituents in preparation thereof as well as content determination method
A technology of active ingredients and determination methods, which is applied in the field of quality control of medicinal materials and their preparations, and can solve the problems of low specificity of quercetin and the like
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Embodiment 1
[0086] Embodiment 1 of the present invention: the preparation method of the reference substance of the active ingredient in the medicinal material of Rhododendron sinensis (see figure 1 ): Dry and pulverize the medicinal materials of the barbarium, reflux and extract with 75% ethanol for 3 times, evaporate the solvent to obtain the extract, disperse the extract with water, and then extract with ethyl acetate and n-butanol, and the ethyl acetate part is repeatedly subjected to silica gel column Chromatography, gradient elution with chloroform-methanol, chloroform-methanol=30:1 part of the extract was concentrated to obtain methyl p-coumarate reference substance; chloroform-methanol=20:1 part of the extract was concentrated to obtain 5-hydroxymethyl Furfural reference substance; the n-butanol part was repeatedly subjected to silica gel column chromatography, and gradient elution was carried out with chloroform-methanol, chloroform-methanol=10:1 part of the extract was concentrat...
Embodiment 2
[0087] Embodiment 2 of the present invention: quercetin-3-O in the medicinal material of Pangui gui -β- The content determination method of D-glucuronic acid: measure according to " Chinese Pharmacopoeia " 2010 edition an appendix VI D high performance liquid chromatography:
[0088] Chromatographic conditions and system suitability test: Octadecyl bonded silica gel as filler; methanol-0.05% phosphoric acid aqueous solution (43:57) as mobile phase; flow rate 1.0mL min -1 ;Column temperature is 30°C; Detection wavelength is 258nm; -β- D-glucuronic acid peak calculation should not be less than 3000;
[0089] Preparation of reference solution: accurately weigh quercetin-3-O -β- Add an appropriate amount of D-glucuronic acid reference substance (prepared in Example 1) to make a solution containing 0.1mg per 1mL;
[0090] Preparation of the test solution: take 0.1 g of the powder of the medicinal material of the bar plate, accurately weigh it, put it in a stoppered conical flask...
Embodiment 3
[0093] Embodiment 3 of the present invention: quercetin-3-O in the medicinal material of guibangui -β- The content determination method of D-glucuronic acid: measure according to " Chinese Pharmacopoeia " 2010 edition an appendix VI D high performance liquid chromatography:
[0094]Chromatographic conditions and system suitability test: Octadecyl bonded silica gel as filler; methanol-0.06% phosphoric acid aqueous solution (40:60) as mobile phase; flow rate 1.0mL min -1 ;Column temperature is 25°C; Detection wavelength is 260nm; -β- D-glucuronic acid peak calculation should not be less than 3000;
[0095] Preparation of reference solution: accurately weigh quercetin-3-O -β- Add appropriate amount of D-glucuronic acid reference substance (made by the applicant), add methanol to make a solution containing 0.01mg per 1mL, and obtain it;
[0096] Preparation of the test solution: take 0.2 g of the powder of the barbaric medicinal material, accurately weigh it, put it in a stoppe...
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