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A kind of preparation method of high-purity sodium pantothenate
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A technology of sodium pantothenate and sodium alanine, applied in the field of medicine, can solve the problems of difficulty, harsh conditions, and long crystal growth time, and achieve the effects of uniform particle size, simple operation and good fluidity
Active Publication Date: 2022-07-08
珠海润都制药股份有限公司
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[0005] The preparation method of sodium pantothenate is mentioned in Chinese patent CN 103145579A: buy commercially available crude sodium pantothenate, dissolve in water, concentrate, decolorize, add a mixed solution of ethanol and ether, cool down and grow crystals in an ultrasonic field for 6 to 12 hours, filter Sodium pantothenate crude drug is obtained. This method is actually a refining method of sodium pantothenate, and requires crystallization and crystallization under an ultrasonic field. The conditions are harsh, the crystallization time is long, labor-consuming, and ether solvents are used, which is dangerous and unsafe. Suitable for industrial production
[0007] Chinese patent CN109280015A uses methanol or ethanol of β-alanine to add sodium methoxide, cools down and adds DL-pantoate lactone, induces resolution, and obtains D-sodium pantothenate with a final yield of about 45%, which is not suitable for industrial production
[0009] Obtaining pure forms of vitamins is tedious and difficult due to the highly lyophilized nature of vitamins, and in these products the purity cannot be They absorb water and thicken when exposed to humidity, making the handling of pantothenic acid formulations a considerable problem
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Embodiment 1
[0032] (1) Preparation of β-alanine sodium
[0033] Add 90kg of isopropanol, 20kg of β-alanine and 9kg of sodium hydroxide into a 200L reaction tank, heat to 60±5°C, and stir for 1-3h. Stop heating, lower the temperature to 5-15°C, and stir to crystallize for 3h. Put the materials in the tank into the centrifuge for centrifugation, collect the filter cake to obtain β-alanine sodium (wet product), dry the wet product at a temperature of 85±5°C for 12 hours, cool to room temperature and collect the material, sample and weigh , get β-alanine sodium, the yield is 95%.
[0034] (2) Preparation of sodium pantothenate (crude product)
[0035] Add isopropanol (11.2 times the weight of β-alanine sodium) to the 500L reaction tank, turn on stirring, add D-pantolactone (1.17 times the weight of β-alanine sodium), add β-propionic acid Sodium sulfamate (full amount in the previous process), heated, temperature controlled at 65±5°C, and reacted for 5h. Stop heating, cool down to 20±5℃, a...
Embodiment 2
[0039] (1) Preparation of β-alanine sodium
[0040] Add 90g anhydrous methanol, 20g β-alanine, 9g sodium hydroxide into a 250ml flask, heat to 62°C, stir for 3h, stop heating, cool down to 10°C, stir for 3h, no crystals are precipitated.
Embodiment 3
[0042] (1) Preparation of β-alanine sodium
[0043] Add 90g absolute ethanol, 20g β-alanine and 9g sodium hydroxide to a 250ml flask, heat to 62°C, stir for 3 hours, stop heating, cool down to 10°C, stir and crystallize for 3 hours, no crystals are precipitated.
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Abstract
The invention discloses a method for preparing high-purity sodium pantothenate. The method uses β-alanine and alkali as raw materials, reacts in a lower alkanol solvent, and prepares sodium β-alanine, β-alanine Sodium and D-pantolactone are reacted in a lower alkanol solvent to obtain a crude product of sodium pantothenate, and the crude product of sodium pantothenate is purified in 95% ethanol and crystallized to obtain sodium pantothenate. The sodium pantothenate prepared by the invention has the advantages of uniform particle size, good fluidity, low hygroscopicity, simple operation, environmental protection, high yield and high purity, and is suitable for industrial production.
Description
technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a preparation method of high-purity sodium pantothenate. Background technique [0002] Pantothenic acid is a B vitamin substance, which is a kind of water-soluble vitamin. It exists widely in the biological world. It is commonly known as vitamin B. (L-form), only the D-form (D-form) has biological activity, and pantothenic acid is commonly used as calcium or sodium salt, which is widely used in medicine, feed, food and other industries. The sodium salt of the enantiomer, because pantothenic acid often needs to be used in combination with other B vitamins such as riboflavin sodium phosphate, it will form calcium phosphate and reduce the potency of the drug and cause incompatibility. Purpose. Therefore, sodium pantothenate is superior to calcium pantothenate in medicinal value and meets the requirements for safe and effective drug use. [0003] Sodium pantothenic ac...
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