Preparation and quality control method of high-purity cinnamon a
A technology of clavenosides and clavenosides is applied in the field of preparation and quality control of high-purity clavenosides A, and can solve the problems of low yield, high production cost, low purity of clavenosides A, and the like, Achieve the effect of fast separation speed, short production cycle and simple and easy method.
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Embodiment 1
[0038] Example 1: Take 5 kg of the leaves of Euphorbiaceae plant stalk flower, crush it into 100 meshes or less, extract 3 times with ethanol with a volume concentration of 50%, filter, combine the filtrate, and recover the ethanol to obtain an ethanol extract to obtain an extract. After silica gel column chromatography, eluted with a chloroform-methanol volume ratio (100:0~95:5) gradient, collect the chloroform-methanol volume ratio (95:5) elution fraction, detect with TCL, and collect the clavicle The fractions of A were combined and concentrated to obtain crude crystals of stalk anthocyanin A. The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: water=22:78; detection wavelength: 255nm; flow rate: 5mL / min), and collect the flowers Glycoside A component, and use HPLC to detect each collected eluate (chromatographic column: C-18 column; mobile phase (volume ratio): acetonitrile: 0.2% phosphoric ...
Embodiment 2
[0039] Example 2: Take 5 kg of the leaves of Euphorbiaceae stalk flower, crush it to below 100 mesh, extract 4 times with 60% ethanol, filter, combine the filtrate, recover the ethanol to obtain the ethanol extract, obtain the extract, and pass it through silica gel Column chromatography, eluted with a gradient of chloroform-methanol (100:0~90:10), collected the elution fraction with a volume ratio of chloroform-methanol (90:10), detected by TCL, collected the fractions containing clavin A , Combined and concentrated to obtain crude crystals of C. The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: water=20:80; detection wavelength: 255nm; flow rate: 5mL / min), and collect the flowers Glycoside A component, and use HPLC to detect each collected eluate (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: 0.2% phosphoric acid solution = 30:70; detection wavelength: 255nm;...
Embodiment 3
[0040] Example 3: Take 5 kg of the leaves of Euphorbia spp. stalk flower, crush it to below 100 mesh, extract 5 times with 80% ethanol, filter, combine the filtrate, recover the ethanol to obtain the ethanol extract, obtain the extract, and pass it through silica gel Column chromatography, eluted with a gradient of chloroform-methanol (100:0~85:15), collected the volume ratio: chloroform-methanol (85:15) elution fraction, detected with TCL, collected the flow containing clavicularin A Separate, combine, and concentrate to obtain crude crystals of C. The crude crystals were prepared by preparative RP-HPLC (chromatographic column: C-18 column; volume ratio: mobile phase: acetonitrile: water=25:75; detection wavelength: 255nm; flow rate: 5mL / min), and collect the flowers Glycoside A component, and use HPLC to detect each collected eluate (chromatographic column: C-18 column; mobile phase: acetonitrile: 0.2% phosphoric acid solution = 40: 60; detection wavelength: 255 nm; flow rate...
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