Method for extracting alkannin naphthoquinone pigment
A technology for naphthoquinones and comfrey, which is applied in the field of extracting naphthoquinone pigments from shikonin, can solve the problems of complicated operation, residual organic solvent, and high extraction cost, and achieves high product quality, natural quality, and high extraction rate. Effect
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Embodiment 1
[0020] Put 10kg of Xinjiang soft comfrey into the extraction kettle of the 24L subcritical fluid extraction process after pulverization, use 1,1,1,2-tetrafluoroethane (R134a) as the extraction agent, the extraction temperature is controlled at 45 ° C, the pressure It is 3.0MPa; the separation temperature is 55°C, the separation pressure is 0.1MPa; the extraction time is 3h. After the extraction was finished, the solvent R134a was recovered, and 676g of crude shkonadhiquinone pigment extract was obtained from the separator.
Embodiment 2
[0022] Send 676g of comfrey extract obtained in the above steps into the film evaporator of molecular distillation uniformly at a rate of 3mL / min using a material pump, heat through the jacket, control the distillation temperature at 60°C, and control the vacuum degree at 30Pa In between, dehydration and desolventization were carried out under the condition that the condensation temperature was 20°C, and 615.8 g of shikonadhoquinone pigment extract was obtained. After analysis, the main several naphthoquinone pigments in this extract were shikonin, Deoxyshikonin, acetylshikonin, dimethylacrylshikonin, isovalerylshikonin, (2-methyl n-butyryl) shikonin, isobutyryl shikonin, etc., naphthoquinone The total content of total pigments is 48.5%.
Embodiment 3
[0024]Take 250 g of the shkonadhiquinone pigment extract obtained in the above-mentioned Example 2 and send it into the distiller of molecular distillation through a delivery pump at a flow rate of 3 mL / min. The distillation temperature is controlled at 90° C., and the vacuum degree is controlled between 3 Pa. Molecular distillation was carried out under the condition that the condensation temperature was 20° C., and the distillate was sent into the product collection tank by the discharge pump to obtain 75.3 g of refined product I. After analysis, the contents of shikonin, deoxyshikonin and acetylshikonin were respectively increased by 58.7%, 43.2%, and 42.1% compared with the directly obtained shikonin extract. The content of valeryl shikonin, (2-methyl n-butyryl) shikonin, isobutyryl shikonin etc. increased by about 10%.
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