Compound salvianolic acid F methyl ester and preparation method thereof
A technology of salvianolic acid and methyl ester, applied in the field of phenolic acid compounds, can solve problems such as unsatisfactory curative effect
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Embodiment 1
[0034] Take 28.7g of crude salvianolic acid (containing not less than 50% salvianolic acid B) and add 1.8L of methanol to dissolve, adjust the pH to 4.5, react under high temperature and high pressure at 120°C for 4 hours, cool down to room temperature, and adjust the pH to 3.0. Recovery of methanol yielded 25.2 g of crude salvianolic acid methyl ester, containing about 11.7% of salvianolic acid methyl ester. The crude total salvianolic acid methyl ester was dissolved in water. Using CG161S reversed-phase resin column (Φ20×50, column bed height 15cm) with 20%-40% methanol gradient elution until phenolic acid F methyl ester appears (collect eluate according to column volume→HPLC quantitative, TLC qualitative detection) to get Salvianolic acid F methyl ester 1.2 grams, content 94.7%.
Embodiment 2
[0036] Take 20 g of total salvianolic acid (salvianolic acid B content 95.0%, HPLC normalization method) and add 1.0 L of methanol to dissolve, adjust the pH to 4.5 with hydrochloric acid, react at high temperature and high pressure at 90 ° C for 5 hours, cool down to room temperature, and adjust the pH to 4.0 . Recover methanol to obtain 15.2 grams of salvianolic acid methyl ester crude product (containing salvianolic acid B; salvianolic acid A; salvianolic acid F and salvianolic acid methyl ester), containing about 21.0% of salvianolic acid methyl ester. The crude total salvianolic acid methyl ester was dissolved in water. Using CG161S reversed-phase resin column (Φ20×50, column bed height 15cm) with 20%-40% methanol gradient elution until phenolic acid F methyl ester appears (collect eluate according to column volume→HPLC quantitative, TLC qualitative detection) to get Salvianolic acid F methyl ester 3.2 grams, content 97.7%.
Embodiment 3
[0038] Take 20 g of total salvianolic acid (salvianolic acid A content 90.2%, HPLC normalization method) and add 1.0 L of methanol to dissolve, adjust the pH to 4, 5 with hydrochloric acid, react under high temperature and high pressure at 120°C for 3 hours, cool down to room temperature, and adjust the pH to 2.0. Recover methanol to obtain the crude salvianolic acid F methyl ester (containing salvianolic acid A; salvianolic acid F and salvianolic acid F methyl ester) 18.2 grams, containing about 31.0% of salvianolic acid F methyl ester. The crude total salvianolic acid methyl ester was dissolved in water. Using CG161S reversed-phase resin column (Φ20×50, column bed height 15cm) with 20%-40% methanol gradient elution until phenolic acid F methyl ester appears (collect eluate according to column volume→HPLC quantitative, TLC qualitative detection) to get Salvianolic acid F methyl ester 6.2 grams, content 97.8%.
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