Determination method of main components of Rheum rhubarb in Shenyanqing tablets
A Shenyanqing tablet content technology, applied to the content detection of emodin and emodin methyl ether in Shenyanqing tablets, in the field of chrysophanol, can solve the problems of backward detection methods, detection methods staying, unaccepted content determination methods, etc. Achieve high sensitivity, easy operation and good reproducibility
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[0027] 3. Preparation of the test solution
[0028] Take the content of Shenyanqing Tablets under the weight difference item, grind or pulverize, mix well, accurately weigh 180mg, put it in a stoppered conical flask, add 10ml of 8% hydrochloric acid solution, dissolve it by ultrasonication, and add 15ml of chloroform , heated to reflux for 1 hour, allowed to cool, placed in a separatory funnel, washed with a small amount of chloroform to wash the stoppered Erlenmeyer flask, incorporated into the separatory funnel, separated to take the chloroform layer, and then extracted the acid solution with chloroform 3 times, 10ml each time, combine the chloroform solution, recover the solvent under reduced pressure to dryness, add methanol to dissolve the residue, transfer to a 10ml measuring bottle, add methanol to the mark, shake well, and filter through a microporous membrane (0.45μm) , that is.
[0029] 4. Blank test
[0030] Take the negative sample of rhubarb lacking soil, operat...
Embodiment 1
[0074] 1. Preparation of Shenyanqing Tablets Astragalus 400g, Motherwort 400g, Imperatae 200g, Liquor 200g, Qumai 200g, Thistle 200g, Shiwei 80g, Burnet Charcoal 60g, Rhubarb 200g, Licorice 20g. Astragalus, add 6 times the amount of water to decoct for 1 hour, filter the decoction and concentrate to a thick paste, and vacuum dry to obtain the dry paste of Astragalus extract. Add 10 times the amount of 65% ethanol to reflux for extraction of rhubarb and small thistle, concentrate the decoction to a thick paste, and dry in vacuum to obtain a dry paste of rhubarb and small thistle extract. Add 6 times the amount of water to decoct the motherwort, Imperata rhizome, Liquor, Qumai, Shiwei, Burnet charcoal, and licorice. The decoction is concentrated to a relative density of 1.1 (60°C), add 3 times the amount of ethanol, and stand for 12 hours Above, filter, and recover ethanol from the filtrate to a thick paste, and vacuum-dry to obtain a dry paste of Qiwei extract. The above three...
Embodiment 2
[0085] The preparation of Shenyanqing tablets and the qualitative determination of the active ingredients of emodin, chrysophanol and emodin methyl ether are the same as in Example 1.
[0086] Determination of Emodin, Chrysophanol and Emodin Methyl Ether in Shenyanqing Tablets
[0087] Chromatographic conditions and system suitability test The chromatographic column is a Dikma Diamonsil C18 column; methanol-0.2% phosphoric acid solution (35:65) is used as the mobile phase; the detection wavelength is 320nm. The number of theoretical plates should not be less than 3000 based on the emodin peak.
[0088] Preparation of Reference Substance Solution Precisely weigh appropriate amounts of emodin reference substance, chrysophanol reference substance, and emodin methyl ether reference substance, and add 80% methanol to prepare each 1ml containing 6 μg of emodin, chrysophanol, and 4 μg of emodin methyl ether solution, mix well, that is.
[0089] Preparation of the test solution Take...
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