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Vincristine purification method

A technology of vincristine and purification method, applied in the field of vincristine purification, can solve problems such as less increase in purity, large solvent consumption, large economic loss, etc., and achieve the effects of stable retention time, reduction of program time, and prevention of solvent effects

Pending Publication Date: 2022-06-07
海南长春花药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the existing vincristine separation and purification process, the main methods are: silica gel column chromatography separation, macroporous resin column chromatography separation, alumina column chromatography separation, these methods are loaded down with trivial details, time-consuming is long, solvent consumption is big, The filler used cannot be reused, is not friendly to the environment, and sometimes requires secondary column or secondary refining, and the purity of vincristine obtained is difficult to reach more than 98%; in addition, there is a method for recrystallization, which is simple to operate, but The purity is less improved and the yield is lower. Due to the low yield and high value of vincristine, the method of recrystallization has a large economic loss

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Embodiment 1

[0056] The present embodiment provides a purification method of vincristine, comprising:

[0057] S10, the preparation of vincristine crude product solution:

[0058] Take 5 g of vincristine crude product (HPLC purity 88.7%), add 50 mL of 60% methanol aqueous solution to dissolve, and adjust the pH to 7.0 with diethylamine. The feed liquid is filtered with a 0.45-micron membrane to obtain a crude vincristine solution for use.

[0059] S20, purification of vincristine:

[0060] Filler bonded phase: C 18 , the particle size is 5 μm.

[0061] Column size: 20mm*250mm.

[0062] Detection wavelength: 297nm.

[0063] Mobile phase: Mobile phase A is 1% diethylamine aqueous solution, adjusted to pH 7.0 with hydrochloric acid,

[0064] Mobile phase B was methanol.

[0065] After installing the preparative column, turn it on and flush the column with 5 column volumes of 60% methanol in water. Equilibrate the column with mobile phase A: mobile phase B=35:65, flow rate 15ml / min, an...

Embodiment 2

[0075] The present embodiment provides a method for purifying vincristine, comprising:

[0076] S10, the preparation of vincristine crude product solution:

[0077] Take 10 g of crude vincristine (HPLC purity 88.7%), add 120 mL of 60% methanol aqueous solution to dissolve, and adjust the pH to 7.3 with diethylamine. The feed liquid is filtered with a 0.45-micron membrane to obtain a crude vincristine solution for use.

[0078] S20, purification of vincristine:

[0079] Filler bonded phase: C 18 , the particle size is 5μm;

[0080] Column specification: 30mm*250mm;

[0081] Detection wavelength: 297nm;

[0082] Mobile phase: Mobile phase A is 3g / L disodium hydrogen phosphate aqueous solution, adjusted to pH 7.3 with phosphoric acid;

[0083] Mobile phase B was methanol.

[0084] After installing the preparative column, turn it on and flush the column with 5 column volumes of 60% methanol in water. Equilibrate the column with mobile phase A: mobile phase B=40:60, flow ra...

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Abstract

The invention discloses a purification method of vincristine, which comprises the following steps: preparation of a vincristine crude product solution: taking a vincristine or vincristine sulfate crude product, adding a solvent for dissolving, adjusting the pH value, and filtering feed liquid to obtain the vincristine crude product solution; purification of vincristine: selecting a chromatographic column, mounting the chromatographic column on a liquid chromatograph, flushing and balancing the chromatographic column by using a mobile phase, performing sample introduction on the vincristine crude product solution, performing gradient elution on the mobile phase, collecting vincristine fractions according to retention time, and repeating sample introduction, elution and collection to obtain vincristine eluent; a filler selected by a chromatographic column is an SPE filler of a silica gel matrix, and bonding phases on the surface of the silica gel are C18, C8 and C6H5; and extraction and concentration of vincristine eluent: carrying out vacuum rotary evaporation on the vincristine eluent, removing an organic phase, adding an organic solvent for extraction, washing an organic layer, and carrying out vacuum rotary drying to obtain a purified vincristine product. The method is convenient to operate, good in durability and repeatability and high in yield, and the purity of the obtained vincristine can reach 99% or above.

Description

technical field [0001] The invention relates to the technical field of medicinal chemical analysis, in particular to a method for purifying vincristine. Background technique [0002] Vincristine is a bisindole alkaloid compound, its target is microtubules, and it mainly inhibits the polymerization of tubulin and affects the formation of spindle microtubules. Stop mitosis in metaphase. It can also interfere with protein metabolism and inhibit the activity of RNA polymerase, and inhibit the synthesis of cell membrane lipids and the transport of amino acids on the cell membrane. Clinically, it is mainly used for the treatment of acute lymphoblastic leukemia, Hodgkin and non-Hodgkin lymphoma, as well as breast cancer, bronchial lung cancer, soft tissue sarcoma and neuroblastoma. [0003] For the existing vincristine separation and purification process, the main methods are: silica gel column chromatography separation, macroporous resin column chromatography separation, alumina...

Claims

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Application Information

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IPC IPC(8): C07D519/04A61P35/00A61P35/02
CPCC07D519/04A61P35/00A61P35/02
Inventor 邓团飞何演安朱义波王亚峰王小力
Owner 海南长春花药业有限公司
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