Method for determining content of mono-ester type alkaloids in monkshood-radix glycyrrhizae medicament
A monoester-type alkaloid and determination method technology, which is applied in the field of pharmaceuticals, can solve the problems of low precision and achieve the effect of good precision and improved tailing factor
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Embodiment 1
[0143] Example 1: Determination of Monoester Alkaloid Content in Fugan Granules
[0144] 1) Preparation of granules: take 6 kg of aconite and 1 kg of licorice, add water to decoct twice, add 8 times the amount of water for the first time, decoct for 2 hours, add 6 times the amount of water for the second time, decoct for 1 hour, combine twice The decoction is filtered, concentrated, dried under reduced pressure, crushed, an appropriate amount of dextrin is added, mixed evenly, granulated by wet method, dried, and granulated to obtain granules of the medicine with sweetener.
[0145] 2) Content determination:
[0146] Chromatographic conditions and system suitability test: chromatographic column (Welch Ulimate Phenyl-Ether, new column) with polar ether linked to phenyl-bonded silica gel as filler; acetonitrile-0.1% phosphoric acid solution=20:80 as mobile phase ; The detection wavelength is 222nm. The number of theoretical plates is 13427 based on the peak of benzoyl aconitin...
Embodiment 2
[0160] Embodiment 2: Determination of monoester type alkaloid content of Fugan Granules
[0161] 1) Preparation of granules: take 18kg aconite and 9kg licorice, add water to decoct twice, add 10 times the amount of water for the first time, decoct for 1.5 hours, add 8 times the amount of water for the second time, decoct for 1 hour, combine twice The decoction is filtered, concentrated, dried under reduced pressure, crushed, an appropriate amount of dextrin is added, mixed evenly, granulated by wet method, dried, and granulated to obtain granules of the medicine with sweetener.
[0162] 2) Content determination:
[0163]Chromatographic conditions and system suitability test: a chromatographic column (Welch Ulimate Phenyl-Ether, used for 2 months) with polar ether linked to phenyl-bonded silica gel as filler; acetonitrile-0.14% phosphoric acid solution=23:77 Mobile phase; detection wavelength is 232nm. The number of theoretical plates is 10141 based on the peak of benzoyl aco...
Embodiment 3
[0170] Embodiment 3: Determination of monoester type alkaloid content of Fugan Granules
[0171] 1) Preparation of granules: Take 10kg of aconite and 5kg of licorice, add water to decoct three times, add 8 times the amount of water for the first time, decoct for 1.5 hours, add 8 times the amount of water for the second time, decoct for 1 hour, and add 6 times the amount of water, decocted for 1 hour, combined three decoctions, filtered, concentrated, dried under reduced pressure, pulverized, added an appropriate amount of dextrin, mixed evenly, wet granulated, dried, and granulated to obtain granules of Fugan drug .
[0172] 2) Content determination:
[0173] Chromatographic conditions and system suitability test: chromatographic column (Venusil XBP Polar-Phenyl, new column) with polar ether-linked phenyl-bonded silica gel as filler; acetonitrile-0.2% phosphoric acid solution=25:75 as mobile phase ; The detection wavelength is 242nm. The number of theoretical plates is 1406...
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