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Purification method for chlorin e6

A chlorin and purification method technology, applied in the field of medicine, can solve the problems of unstable process, high equipment requirements, complex chlorophyll a extraction and purification process, etc., and achieve high purification efficiency, simple and stable process operation, and enhanced solubility. Effect

Pending Publication Date: 2021-03-19
康俄(上海)医疗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction and purification process of chlorophyll a in this patent is complicated, requiring high-speed centrifuge, extremely low temperature (-20°C) and other conditions, and the purity of the prepared sodium salt of chlorin e6 depends on the purity of chlorophyll a and the preparation process
Therefore, this method has the disadvantages of high equipment requirements, unsuitable for scale-up production, unstable process, etc.

Method used

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  • Purification method for chlorin e6
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  • Purification method for chlorin e6

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: Salt formation of chlorin e6 and meglumine

[0031] Under the protection of argon, add 200g of crude chlorin e6 into 1L of tetrahydrofuran, heat to 50-60°C, and stir to dissolve. Add 196.31 g of meglumine, stir for 1 h, then lower the temperature to 0-10° C. and crystallize for 2 h. Filter, rinse the filter cake with 200mLTHF, and dry to obtain 357.07g of chlorin e6 meglumine salt, with a yield of 90.10%.

Embodiment 2

[0032] Example 2: Dissociation of chlorin e6 meglumine salt

[0033] Under argon protection, 350g of chlorin e6 meglumine salt in Example 1 was dissolved in a mixed solution of 1L of tetrahydrofuran and water, cooled to 0-10°C, and 10% hydrochloric acid solution was added dropwise to adjust the pH= 3-4, more solids were precipitated, continued to stir and crystallize for 2 hours, filtered, washed the filter cake with 350ml of water, and dried in vacuo to obtain 168.15g of chlorin e6 with a yield of 95.20%.

Embodiment 3

[0034] Embodiment 3: Salt formation of chlorin e6 and ethanolamine

[0035] Under the protection of argon, add 100g of crude chlorin e6 into 1.20L of acetone, heat to 50-60°C, and stir to dissolve. Add 30.71g of ethanolamine, stir for 2h, then cool down to 0-10°C for crystallization for 2h. Filter, rinse the filter cake with 50 mL of acetone, and dry to obtain 117.26 g of chlorin e6 ethanolamine salt, with a yield of 89.71%.

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Abstract

The invention belongs to the field of medicines, and particularly relates to a purification method for chlorin e6 . The purification method comprises the following steps: addition of alkali for salt formation and addition of acid for dissociation. The purification method comprises the following specific steps: namely dissolving a crude chlorin e6 product into a salt-forming solvent, adding alkalito form salt, conducting crystallizing and filtering, then dissolving a filter cake into a dissociation solvent, adding acid for dissociation, and performing crystallizing to obtain high-purity chlorin e6. The method has the advantages of simple and stable process operation and high purification efficiency.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a method for purifying chlorin e6. Background technique [0002] Photodynamic therapy is another new technology for tumor treatment after surgery, radiotherapy and chemotherapy. The basis of its treatment is to irradiate the tumor tissue enriched with photosensitizer with a certain wavelength of light, and the photosensitizer induces photodynamic and other effects, resulting in tumor tissue necrosis and showing therapeutic effect. Studies have shown that chlorin e6 has a reliable photodynamic effect on mouse solid sarcoma-180 transplanted tumors. Compared with photosensitizers currently used clinically at home and abroad, it has a clear chemical structure and a higher absorption coefficient in the red light treatment area. Porphyrin preparations are an order of magnitude higher, have strong photosensitivity, and have the characteristics of fast clearance in the body and low t...

Claims

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Application Information

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IPC IPC(8): C07D487/22A61K41/00A61P35/00
CPCC07D487/22A61K41/0071A61P35/00
Inventor 吴思丹李亮庞玉华张涛黄羽莎肖峰平宋治国
Owner 康俄(上海)医疗科技有限公司
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