CN109111493B - Raw material refining method for preparing troxerutin for injection - Google Patents
Raw material refining method for preparing troxerutin for injection Download PDFInfo
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- CN109111493B CN109111493B CN201811189729.2A CN201811189729A CN109111493B CN 109111493 B CN109111493 B CN 109111493B CN 201811189729 A CN201811189729 A CN 201811189729A CN 109111493 B CN109111493 B CN 109111493B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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Abstract
The invention discloses a raw material refining method for preparing troxerutin for injection, which comprises the following specific steps: adding rutin and purified water into a reaction kettle according to a certain mass ratio, stirring and heating to over 70 ℃, keeping the temperature, stirring and washing, filtering, washing a filter cake with purified water, and drying to obtain the raw material rutin of troxerutin for injection; if the obtained raw material rutin does not meet the preparation requirement of troxerutin for injection, the obtained raw material rutin is refined again according to the method. The method has the advantages of simple operation, easy industrial production and high yield, and the single refining weight yield is more than 95%.
Description
Technical Field
The invention belongs to the technical field of troxerutin preparation for injection, and particularly relates to a raw material refining method for preparing troxerutin for injection.
Background
Troxerutin (troxerutin) is yellow or yellowish green powder, has odorless and hygroscopic effects, is mainly used for anticoagulant, has effect of preventing thrombosis, and is suitable for hemiplegia, aphasia, myocardial infarction, arteriosclerosis, etc. caused by cerebral thrombosis and cerebral embolism.
According to the standard of Chinese pharmacopoeia, troxerutin related substances for injection specify that a troxerutin peak, a dihydroxyethylrutin peak and a tetrahydroxyethylrutin peak are not more than 5.0 percent of the total peak area, the peak area of other single unknown components is not more than 1.0 percent of the total peak area, the sum of the peak areas of the unknown components is not more than 4.0 percent of the total peak area, and the sum of the peak areas of the components is not more than 12.0 percent of the total peak area (for injection). However, rutin is taken as a starting material, in the process of preparing troxerutin for injection, two impurities brought in the rutin directly influence the content of related substances in a finished product, according to the detection method of the troxerutin related substances, the relative retention time of the impurity 1 in the rutin is 1.20-1.40, the relative retention time of the impurity 2 in the rutin is 1.40-1.70, the peak area of a single unknown component is always larger than 1.0% due to the impurity 1 and the impurity 2, and the sum of the peak areas of the unknown components is larger than 4.0%.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a raw material refining method for preparing troxerutin for injection, which is simple to operate, easy to realize industrial production and high in yield.
The purpose of the invention is realized as follows: a raw material refining method for preparing troxerutin for injection comprises the following steps: adding rutin and purified water into a reaction kettle according to a certain mass ratio, stirring and heating to over 70 ℃, keeping the temperature, stirring and washing, filtering, washing a filter cake with purified water, and drying to obtain the raw material rutin of troxerutin for injection; if the obtained raw material rutin does not meet the preparation requirement of troxerutin for injection, the obtained raw material rutin is refined again according to the method.
Preferably, the mass ratio of the rutin to the purified water is 1: 5-12, and preferably 1: 8.
Preferably, the temperature of the heat preservation stirring washing is 70-100 ℃, and preferably 90-100 ℃.
Preferably, the heat-preservation stirring and washing time is 0.5-2 hours, preferably 1 hour.
Preferably, the temperature of the purified water for washing is 0-100 ℃, and preferably 60-100 ℃.
Preferably, when the obtained raw material rutin can not meet the preparation requirement of troxerutin for injection, refining for 2-4 times according to the method.
Due to the adoption of the technical scheme, the invention has the beneficial effects that: the method is simple to operate, easy to realize industrial production, and the obtained raw material rutin product has good quality, high yield and low impurity content, and completely meets the preparation requirement of troxerutin for injection.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments.
Example 1:
weighing 150g of rutin (the impurity 1 is 1.063 percent and the impurity 2 is 1.345 percent) and 1200g of purified water, adding the rutin and the purified water into a reaction bottle, stirring and heating to reflux, keeping the temperature and stirring for 1 hour, filtering, rinsing the filter cake with the purified water with the temperature of more than 80 ℃, collecting the filter cake, and drying to obtain 146.4g of refined rutin, wherein the weight yield is 97.6 percent, the impurity 1 is 0.925 percent and the impurity 2 is 0.778 percent.
Example 2:
weighing 150g of rutin (detected as 1.24% of impurity 1 and 1.43% of impurity 2) and 1200g of purified water, adding the rutin and the purified water into a reaction bottle, stirring and heating to reflux, keeping the temperature and stirring for 1 hour, filtering, rinsing a filter cake with the purified water with the temperature of more than 80 ℃, collecting the filter cake, and drying to obtain 144.3g of refined rutin, wherein the weight yield is 96.2%, the impurity 1 is 1.105%, and the impurity 2 is 0.903%.
Example 3:
weighing 144.3g of rutin (detected as 1.105% of impurity 1 and 0.903% of impurity 2) and 1200g of purified water, adding the rutin and the 1200g of purified water into a reaction bottle, stirring and heating to reflux, keeping the temperature and stirring for 1 hour, filtering, rinsing the filter cake with the purified water with the temperature of more than 80 ℃, collecting the filter cake, and drying to obtain 139.9g of refined rutin, wherein the weight yield is 97.0%, the impurity 1 is 0.956%, and the impurity 2 is 0.605%.
In the above embodiment, the starting material rutin and the refined rutin obtained by refining according to the method are detected according to a detection method of related substances of troxerutin in second part of 2015 edition Chinese pharmacopoeia, and then the contents of impurity 1 and impurity 2 are calculated according to a peak area normalization method.
Therefore, the method is simple to operate, industrial production is easy to realize, the obtained raw material rutin product is good in quality and high in yield, the single refining weight yield is over 95%, the impurity content is low, and the preparation requirement of troxerutin for injection is completely met.
Finally, it should be noted that the above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and although the present invention is described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the specific embodiments of the present invention without departing from the spirit and scope of the present invention, and all the modifications or equivalent substitutions should be covered in the claims of the present invention.
Claims (2)
1. A raw material refining method for preparing troxerutin for injection is characterized by comprising the following steps: adding rutin and purified water into a reaction kettle according to a certain mass ratio, wherein the mass ratio of the rutin to the purified water is 1: 5-12, stirring and heating to above 70 ℃, refluxing, keeping the temperature, stirring and washing, wherein the temperature for keeping the temperature and stirring and washing is 70-100 ℃, the time for keeping the temperature and stirring and washing is 0.5-2 h, filtering, washing a filter cake with the purified water, wherein the temperature for washing is 0-100 ℃, and drying to obtain the raw material rutin of troxerutin for injection; if the obtained raw material rutin does not meet the preparation requirement of troxerutin for injection, the obtained raw material rutin is refined again according to the method.
2. The refining method of raw materials for preparing troxerutin for injection according to claim 1, characterized in that: when the obtained raw material rutin can not meet the preparation requirement of troxerutin for injection, refining for 2-4 times according to the method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811189729.2A CN109111493B (en) | 2018-10-12 | 2018-10-12 | Raw material refining method for preparing troxerutin for injection |
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| CN201811189729.2A CN109111493B (en) | 2018-10-12 | 2018-10-12 | Raw material refining method for preparing troxerutin for injection |
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| CN109111493A CN109111493A (en) | 2019-01-01 |
| CN109111493B true CN109111493B (en) | 2021-08-10 |
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| CN117264002A (en) * | 2023-11-22 | 2023-12-22 | 成都欧康医药股份有限公司 | Preparation method and application of high-purity and high-content rutin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923139A (en) * | 2014-05-08 | 2014-07-16 | 徐大鹏 | Method for extracting rutin from sophora flower buds |
| CN105541776A (en) * | 2016-03-08 | 2016-05-04 | 张婷婷 | Method for extracting rutin from Japanese pagodatree flower buds and preparing quercetin |
| CN106892950A (en) * | 2017-03-02 | 2017-06-27 | 河南师范大学 | A kind of preparation method of high-content troxerutin |
| CN107434816A (en) * | 2016-05-25 | 2017-12-05 | 辽宁药联制药有限公司 | One kind extracts rutin method from Ilex Latifolia Thunb |
| CN107827941A (en) * | 2017-11-25 | 2018-03-23 | 衡阳县华盛达农林科技有限公司 | Rutin extraction method |
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2018
- 2018-10-12 CN CN201811189729.2A patent/CN109111493B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923139A (en) * | 2014-05-08 | 2014-07-16 | 徐大鹏 | Method for extracting rutin from sophora flower buds |
| CN105541776A (en) * | 2016-03-08 | 2016-05-04 | 张婷婷 | Method for extracting rutin from Japanese pagodatree flower buds and preparing quercetin |
| CN107434816A (en) * | 2016-05-25 | 2017-12-05 | 辽宁药联制药有限公司 | One kind extracts rutin method from Ilex Latifolia Thunb |
| CN106892950A (en) * | 2017-03-02 | 2017-06-27 | 河南师范大学 | A kind of preparation method of high-content troxerutin |
| CN107827941A (en) * | 2017-11-25 | 2018-03-23 | 衡阳县华盛达农林科技有限公司 | Rutin extraction method |
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