Process for preparing Danshensu
A technology of danshensu and salvia miltiorrhiza, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of conflicting purity, yield and processing capacity, low processing capacity, high cost, etc., and achieve low cost and high recovery rate High, guaranteed separation performance
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[0031] Example 1
[0032] 1. Crushing and degreasing
[0033] 2 kg of salvia root → crushed (1~3mm) → degreasing with petroleum ether (4L×3) → drying → defatted salvia miltiorrhiza powder.
[0034] 2: Extraction, ultrafiltration, concentration
[0035] Defatted salvia powder→16L deionized water extraction (80℃, 2 hours)→12L deionized water extraction (80℃, 2 hours)→8L deionized water extraction (80℃, 2 hours)→combination→ultrafiltration→decompression Concentrate to 2L.
[0036] 3: Conversion
[0037] Salvia miltiorrhiza concentrate → add sodium bisulfite (10g) and saturated NaOH to adjust to pH 9-10 → stir under nitrogen protection for 2 hours → add 2 mol.L -1 HCl to adjust the pH to 3.0.
[0038] 4: Extraction
[0039] Acidified Danshen transformation solution → ethyl acetate extraction (600 mL×5) → ethyl acetate recovery under reduced pressure → crude Danshensu (18 g, light yellow powder, Danshensu purity 65%, protocatechuic aldehyde 16%).
[0040] 5: Silica gel chrom...
Example Embodiment
[0042] Example 2
[0043] 1: Extraction, ultrafiltration, concentration
[0044] Salvia Root 100kg→Pulverization (1~3mm)→800L Deionized Water Extraction (80℃, 2 Hours)→600L Deionized Water Extraction (80℃, 2 Hours)→400L Deionized Water Extraction (80℃, 2 Hours) →Merge →Ultrafiltration →Concentrate under reduced pressure to 100L.
[0045] 2: Conversion
[0046] Salvia miltiorrhiza concentrate → add sodium bisulfite (500g) and saturated NaOH to adjust pH to 9-10 → stir under nitrogen protection for 2 hours → add 2 mol.L -1 HCl to adjust the pH to 3.0.
[0047] 3: Extraction
[0048] Acidified Danshen transformation solution→ethyl acetate extraction (30L×5)→recovery of ethyl acetate under reduced pressure→crude Danshensu (920 g, light yellow powder, Danshensu purity 67%, protocatechuic aldehyde 14%).
[0049] 4: Silica gel chromatography
[0050] Crude Danshensu (920g)→adding diatomite (2.5kg) and mixing→vacuum drying→solid powder→put on stainless steel column (silica gel 20k...
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