Method for preparing salvianolic acid A by catalytically converting salvianolic acid B
A technology of salvianolic acid and displacement chromatography, applied in the field of catalytic conversion of salvianolic acid B to prepare salvianolic acid A, can solve the problems of low conversion rate, increased equipment investment, reagent and artificial energy consumption, low separation and purification yield, etc. , to achieve the effect of increasing the yield and shortening the time of the fragile state
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Embodiment 1
[0038] Step 1: Resin Treatment
[0039] Put the ADS-5 and HPD100 macroporous adsorption resins used in this process into their respective chromatographic columns → add acetone to submerge the resin → vacuum degas → elute with acetone until the outflow of acetone is clear → elute with 95% ethanol until the outflow of ethanol without adding water Turbidity is the standard → eluted with deionized water until the effluent has no alcohol smell (generally 5 column volumes for elution) → soak in 4% NaOH overnight → eluted with 4% NaOH for 2 column volumes (BV) → wash with deionized water Remove to neutral → 4% HCl soak overnight → 4% HCl elution 2BV → deionized water elution to neutral (both flow rates are 2cm / min).
[0040] Step 2: Extraction of salvianolic acid B
[0041] Salvia miltiorrhiza (containing salvianolic acid B 6.1%)→dried, crushed and sieved (40 mesh, 40 kg)→water extraction (100°C, 480L×3)→water extract (2318 grams of salvianolic acid B, content 11.36%) , the total s...
Embodiment 2
[0047] Step 4: Crude salvianolic acid B (2.8g, 65.3% SB) → dissolve in 180mL water → add urea (0.08g, about 0.5 moles of salvianolic acid B) → dissolve → transform at 120°C for 4 hours → reduce to room temperature → Adjust pH to 3.0→salvianolic acid B conversion liquid [2.9 grams of solid total weight, containing 19% of salvianolic acid A, 0.56 grams in total, yield 30% (conversion rate 45%)].
[0048] Other steps are with embodiment 1.
Embodiment 3
[0050] Step 4: Crude salvianolic acid B (2.8g, 65.3% SB) → dissolve in 180mL water → add urea (0.05g, about 0.3 moles of salvianolic acid B) → dissolve → transform at 110°C for 4 hours → drop to room temperature → Adjust pH to 3.0→salvianolic acid B conversion solution [2.82 grams of solid total weight, containing 8.86% of salvianolic acid A, 0.25 grams in total, yield 13.67% (conversion rate 20%)].
[0051] Other steps are with embodiment 1.
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