Preparation method of ajoene
A technology of ajoene and evaporation surface, which is applied in the field of preparation of ajoene from plants, can solve the problems that there is no report on the preparation process for industrialized large-scale production of high-purity ajoene, and achieve the benefits of large-scale production operations and low energy consumption. Small, less polluting effect
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Embodiment 1
[0023] Take 10Kg of garlic bulbs, crush them, and add them to CO 2 In the supercritical extractor, the extraction pressure is 10MPa, the temperature is 35°C, CO 2 The flow rate is 1ml / g crude drug·min, the extraction time is 80min, and CO 2 Supercritical extract; added to molecular still for three-stage molecular distillation, wherein the evaporation surface temperature of the first stage distillation is 100°C, the pressure is 90Pa, the distillation time is 80min, the distillate is collected, and the second stage distillation is carried out, evaporated The surface temperature is 60°C, the pressure is 90Pa, distilled for 80min, the distillate is collected, and the third stage distillation is carried out, the evaporation surface temperature is 30°C, the pressure is 90Pa, the distillate is collected for 70min, and the oily ajoene is obtained. 10.3g, detected by HPLC, the purity is 91.6%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are co...
Embodiment 2
[0025] Take 10Kg of garlic bulbs, crush them, and add them to CO 2 In the supercritical extractor, the extraction pressure is 30MPa, the temperature is 50°C, CO 2 The flow rate is 4ml / g crude drug·min, the extraction time is 120min, and CO 2 Supercritical extract; added to molecular still for three-stage molecular distillation, wherein the evaporation surface temperature of the first-stage distillation is 150°C, the pressure is 150Pa, and the distillation time is 80min, the distillate is collected, and the second-stage distillation is carried out to evaporate The surface temperature is 90°C, the pressure is 150Pa, distilled for 80min, the distillate is collected, and the third stage distillation is carried out. The evaporation surface temperature is 50°C, the pressure is 150Pa, and the distillate is collected for 70min, and the distillate is obtained to obtain the oily ajoene 14.3g, detected by HPLC, the purity is 90.3%, UV, IR, MS, 2 HNMR, 13 The data characterizing its ph...
Embodiment 3
[0027] Take 10Kg of garlic bulbs, crush them, and add them to CO 2 In the supercritical extractor, the extraction pressure is 20MPa, the temperature is 40°C, CO 2 The flow rate is 3ml / g crude drug·min, the extraction time is 100min, and CO 2 Supercritical extract; added to molecular still for three-stage molecular distillation, wherein the evaporation surface temperature of the first stage distillation is 120°C, the pressure is 100Pa, the distillation time is 80min, the distillate is collected, and the second stage distillation is carried out, evaporated The surface temperature is 80°C, the pressure is 100Pa, distilled for 80min, the distillate is collected, and the third stage distillation is carried out. The evaporation surface temperature is 40°C, the pressure is 100Pa, distilled for 70min, and the distillate is collected to obtain the oily ajoene 10.8g, detected by HPLC, the purity is 95.1%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as ...
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