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Method for preparing high-purity stigmasterol from phytosterol oleate

A technology of phytosterol oleate and stigmasterol oleate, which is applied in the direction of steroids and organic chemistry, can solve the problems of many times of crystallization and complicated process, and achieve simple operation steps, full utilization and less times of crystallization Effect

Active Publication Date: 2018-02-23
XIAN HEALTHFUL BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above processes all use phytosterols as raw materials to prepare stigmasterol, and the crystallization times are many and the process is complicated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Freezing separation

[0025] Dissolve 200kg of phytosterol oleate (the content of stigmasterol is 15.58%) in 1000L ethyl acetate, stir at 65°C until the phytosterol oleate is completely dissolved, then transfer it to a freezer and freeze it at -20°C Freeze for 8 hours. The clear liquid obtained by freezing separation was subjected to vacuum distillation to recover ethyl acetate to obtain 32.71 kg of crude stigmasterol oleate.

[0026] 2. Saponification reaction

[0027] Add 300 L of 5% NaOH ethanol solution with a mass fraction of 300 L to the crude stigmasterol oleate obtained in step 1, and carry out saponification reaction at 80° C., and the reaction time is 4 hours.

[0028] 3. Solid-liquid separation

[0029] After the saponification reaction, add 300L NaCl saturated aqueous solution to the saponification liquid, and wait until sodium oleate is completely precipitated from the saponification liquid, and use a tympanic filter press to separate the saponificati...

Embodiment 2

[0035] 1. Freezing separation

[0036] Dissolve 100g of phytosterol oleate (the content of stigmasterol is 15.58%) in 400mL of ethyl acetate, stir and dissolve at 65°C until the phytosterol oleate is completely dissolved, then transfer it to a freezer, and store it at -20 Freeze and separate at ℃ for 10 hours. The clear liquid obtained by freezing separation was subjected to vacuum distillation to recover ethyl acetate to obtain 18.57 g of crude stigmasterol oleate.

[0037] 2. Saponification reaction

[0038] Add 185 mL of 5% NaOH ethanol solution to the crude product of stigmasterol oleate obtained in step 1, and carry out saponification reaction at 80° C., and the reaction time is 3 hours.

[0039] 3. Solid-liquid separation

[0040] After the saponification reaction, add 185mL NaCl saturated aqueous solution to the saponification solution, and wait until sodium oleate is completely precipitated from the saponification solution, use a tympanic filter press to separate th...

Embodiment 3

[0046] 1. Freezing separation

[0047] Dissolve 100g of phytosterol oleate (the content of stigmasterol is 15.58%) in 800mL of ethyl acetate, stir at 60°C until the phytosterol oleate is completely dissolved, then transfer it to a freezer, and freeze it at -20°C Freeze for 5 hours. The clear liquid obtained by freezing separation was subjected to vacuum distillation to recover ethyl acetate to obtain 19.38 g of crude stigmasterol oleate.

[0048] 2. Saponification reaction

[0049] Add 95 mL of 8% NaOH ethanol solution with a mass fraction of 8% to the crude stigmasterol oleate obtained in step 1, and carry out saponification reaction at 80° C. for 5 hours.

[0050] 3. Solid-liquid separation

[0051] After the saponification reaction, add 190mL NaCl saturated aqueous solution to the saponification solution, and wait until sodium oleate is completely precipitated from the saponification solution, use a tympanic filter press to separate the saponification product at 6kPa to ...

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PUM

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Abstract

The invention discloses a method for preparing high-purity stigmasterol from phytosterol oleate. The method comprises the following steps of taking phytosterol oleate as a raw material, and performingsubzero fractionation, saponification, solid-liquid separation and two times of crystallization and purification to obtain a stigmasterol product with purity equal to 95% or more. Compared with the prior art, in the method, the phytosterol oleate is taken as the raw material to prepare the high-purity stigmasterol, the method has fewer crystal number of times and is simple in operation steps, thesolvent used for crystallization and purification can be recycled, making full use of resources is realized, and the production cost is lowered.

Description

technical field [0001] The invention belongs to the technical field of preparation of stigmasterol, and in particular relates to a method for preparing high-purity stigmasterol from phytosterol oleate. Background technique [0002] Natural phytosterols are similar in structure to animal sterols such as cholesterol. They are an active ingredient in plants. They exist in various vegetable oils and are widely used in medicine, food, cosmetics and other industries. The main components of phytosterols include campesterol, β-sitosterol, stigmasterol and brassicasterol. Brassinolide is a plant green growth regulator, and its market capacity in 2017 will be about 1 billion. Due to its structural characteristics, stigmasterol can be used as a raw material for the synthesis of brassinolide, and has been favored by domestic and foreign markets. extensive attention. At the same time, because of its unique physiological functions, stigmasterol can be used as synthetic sex hormones, adr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
CPCC07J9/00
Inventor 李青孟永宏李玉松孟利军
Owner XIAN HEALTHFUL BIOTECH
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