Production process for preparing high-purity synephrine by crystallization method

A production process and crystallization technology, which are applied in the production process field of preparing high-purity synephrine by crystallization, can solve the problems of high energy consumption cost, insufficient purity, complicated process, etc., and achieve a high degree of continuous production and high extraction efficiency. Simple method and high solvent utilization effect

Active Publication Date: 2018-06-29
MIANYANG DIAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the purity of the synephrine freeze-dried powder produced by this process is relatively high, it also involves more raw materials, the process is complicated, and there are also the following problems: the process uses an organic solvent and adds an alkaline reagent to heat and extract, and the cost is high , high pollution, and synephrine is greatly damaged by heating under alkaline conditions, and long-term extraction will reduce the extraction yield of synephrine; in the separation and purification process, the decolorization process utilizes mixed organic solvent extraction. On the one hand, These solvents need to be recycled and reused. The recovery and rectification of organic solvents consume a lot of steam, and the energy cost is high. On the other hand, the recycled mixed organic solvents will remove impurities due to their respective physical characteristics. The effect of the product will be affected, resulting in the instability of the product content, and the extraction is based on the interaction of positive and negative charges. In the actual operation process, the positively charged small molecules such as amino acids and vitamins contained in the synephrine solution will also be extracted Remove and destroy its performance; the crystallization process of the product is the concentrated ice bath crystallization method, the concentration of the concentrated solution, the concentration temperature and the concentration time in this method all have an impact on the content of synephrine, the product content is unstable, and the ice bath crystallization A refrigerator is required, which increases production costs
[0005] In summary, the synephrine preparation process in the prior art has the problems of complex process, many raw materials involved, high energy consumption, unstable and insufficient purity of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0045] Take 100kg of Citrus aurantium raw material, pulverize and moisten it, percolate and extract with dilute hydrochloric acid with a concentration of 0.02mol / L and a volume of 500L to obtain an extract; after adsorbing the extract with a 732 cation exchange resin with a volume of 100L, use the mass concentration Analyze 5% of dilute ammonia water with a volume of 500L to obtain synephrine analytical solution; concentrate the analytical solution at room temperature under vacuum under reduced pressure to obtain synephrine crude extract, and at the same time recover ammonia; use water as a solvent to refine the crude extract and add Adjust the pH to 1 with dilute hydrochloric acid, and then add 8kg of activated carbon to decolorize and filter to obtain a decolorizing liquid; add 3% sodium hydroxide to pH=7 by mass concentration to the decolorizing liquid, leave to crystallize, filter, wash, and dry to obtain a purity of 98.2 % Synephrine product; the filtrate is then adsorbed b...

example 2

[0047] Take 100kg of Citrus aurantium raw material, crush and moisten it, percolate and extract with dilute hydrochloric acid with a concentration of 0.01mol / L and a volume of 700L to obtain an extract; after adsorbing the extract with a 732 cation exchange resin with a volume of 240L, use the mass concentration Analyze 4% dilute ammonia water with a volume of 700L to obtain synephrine analytical solution; concentrate the analytical solution at room temperature under vacuum under reduced pressure to obtain synephrine crude extract, while recovering ammonia water; refine the crude extract with water as a solvent and add Adjust the pH to 5 with dilute hydrochloric acid, and then add 5kg of activated carbon to decolorize and filter to obtain a decolorizing solution; add 6% by mass sodium hydroxide to the decolorizing solution to pH=9, stand for crystallization, filter, wash, and dry to obtain a purity of 97.9 % Synephrine product; the filtrate is then adsorbed by 732 cation exchang...

example 3

[0049] Take 100kg of Citrus aurantium raw material, pulverize and moisten it, percolate and extract with dilute hydrochloric acid with a concentration of 0.05mol / L and a volume of 600L to obtain an extract; after adsorbing the extract with a 732 cation exchange resin with a volume of 200L, use the mass concentration Dilute ammonia water with a volume of 9% and a volume of 600L was analyzed to obtain synephrine analytical solution; the analytical solution was concentrated under vacuum and reduced pressure at room temperature to obtain crude synephrine extract, while ammonia water was recovered; the crude extract was refined with water as a solvent and added Adjust the pH to 5 with dilute hydrochloric acid, and then add 5kg of activated carbon to decolorize and filter to obtain a decolorizing solution; add 5% by mass sodium hydroxide to the decolorizing solution to pH=9, stand for crystallization, filter, wash, and dry to obtain a purity of 97.7 % Synephrine product; the filtrate ...

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Abstract

The invention relates to a production process for preparing synephrine, in particular to a production process for preparing high-purity synephrine by using a crystallization method. The production process comprises the following steps: by taking trifoliate oranges in the market as a raw material, extracting by using a strong-acid solvent, adsorbing by using cation exchange resin, performing ammonia water dissolution, concentrating, refining by using water as a solvent, performing normal-temperature decoloring by using activated carbon, filtering, crystallizing, filtering crystalline, washing, and drying at normal pressure and at 85 DEG C, thereby obtaining a synephrine product. The purity of the synephrine product prepared by using the production process can be 98% or above, and meanwhile, a synephrine product of which the purity is up to 70% can be recycled; the synephrine product prepared by using the production process is good in stability and easy to preserve, and meanwhile, the production process is simple, small in number of used equipment, convenient to operate, low in cost and very applicable to industrial production.

Description

Technical field [0001] The invention relates to a production process for preparing synephrine, in particular to a production process for preparing high-purity synephrine by using a crystallization method. Background technique [0002] Synephrine is mainly derived from the dried young fruit of the Rutaceae plant Lime, among them, because the main component of Citrus aurantium is alkaloids, and this alkaloid is mainly synephrine, so it is widely used to extract synephrine . Synephrine's pharmacological effects are mainly manifested in the effects of raising blood pressure, oxidizing fat, lowering blood lipids, constricting blood vessels, strengthening the heart, and diuresis. It is a natural stimulant with no side effects. It is mainly used for the treatment of bronchial asthma and hypotension in clinic. , Collapse and shock, food failure, gastroptosis, etc. In addition, synephrine also has the effect of improving metabolism and increasing calorie consumption. Therefore, synephr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/10C07C215/60
CPCC07C213/10C07C215/60
Inventor 周传武江波
Owner MIANYANG DIAO PHARMA
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