A kind of preparation method of 6,7-epoxy ligustilide
The technology of ligustilide and epoxy is applied in the field of preparation of chemical components of traditional Chinese medicine, can solve the problems of expensive raw materials, cumbersome steps, difficult to prepare in large quantities, etc. Effect
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Embodiment 1
[0026] A kind of preparation method of 6,7-epoxy ligustilide, its steps are:
[0027] (1) Reaction: Add 100ml of water-ethanol (25:75, v / v) and 5g of volatile oil of Ligusticum chuanxiong (Ligustilide content 19.5%, w / w) into a 250ml round bottom flask in sequence, and stir at room temperature for 5 minutes. Take 10g of potassium hydrogen persulfate compound salt, slowly add it to the reaction system, stir at room temperature for 5 minutes, then place it in a water bath at 80°C for reaction, and stop the reaction when the chromatographic peak area of ligustilide in the reaction solution is detected to decrease by 75%. ;
[0028] (2) Detection: Waters Acquity UPLC chromatograph; chromatographic column Waters BEH C18 (50mm×2.1mm, 1.7μm); mobile phase acetonitrile (A)–0.1% phosphoric acid water (B); gradient elution 0~0.5min (20 % A), 0.5~3.0min (20% A~70% A), 3.0-3.5min (70% A~100% A), 3.5~4.0min (100% A), 4.0~4.01min (100% A ~20% A), 4.01~5.0min (20% A); flow rate 0.4ml / min...
Embodiment 2
[0032] A kind of preparation method of 6,7-epoxy ligustilide, its steps are:
[0033] (1) Preparation of angelica extract: 1 kg of angelica medicinal material, crushed, passed through a No. 3 sieve, extracted by steam distillation, and 5.7 g of angelica volatile oil was obtained;
[0034] (2) Reaction: Add 40 ml of water-1,4-dioxane (10:90, v / v), 2 g of angelica volatile oil prepared in step (1) (42.1% ligustilide content, w / w) Add to a 100 ml round-bottomed flask one by one, and stir at room temperature for 5 minutes. Take 9 g of potassium hydrogen persulfate compound salt, slowly add it to the reaction system, stir at room temperature for 5 minutes, and then place it in a water bath at 100°C for reaction; the reaction process is monitored by liquid chromatography, and the peak area of ligustilide in the reaction solution is The reaction is terminated when it is reduced by 85%;
[0035] (3) Separation: After the reaction, remove the insoluble matter by suction filtration...
Embodiment 3
[0037] A kind of preparation method of 6,7-epoxy ligustilide, its steps are:
[0038] Add 20 ml of water-methanol (5:95, v / v) and 0.5 g of crude ligustilide (content 80%, w / w) into a 50 ml round bottom flask in sequence, and stir at room temperature for 5 minutes; Slowly add 3 g of potassium bisulfate compound salt into the reaction system, stir at room temperature for 10 minutes, and then react in a water bath at 50°C; the reaction process is monitored by liquid chromatography, and the peak area of ligustilide in the reaction solution is reduced by 80% After the reaction, the insoluble matter was removed by suction filtration, the filtrate was concentrated under reduced pressure at 40°C to remove the solvent, and the residue was separated by pressurized silica gel column chromatography (φ30 mm×200 mm), and the mobile phase was petroleum ether-ethyl acetate (6:1, v / v), fractions were collected at 20ml / part; the fractions were combined after UPLC detection, and the solvent wa...
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