Method for purifying Vinorelbine Bitartrate

A technology of vinorelbine and a new method, applied in the field of purifying vinorelbine, can solve the problems of low efficiency, inability to carry out industrial production, and less purification amount.

Inactive Publication Date: 2005-11-16
NORTHEAST FORESTRY UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of separation and purification, Lin Yongjiang et al. separated the crude Vinorelbine synthesized by positive pressure column chromatography twice, and obtained the product with

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take a hollow PVC column with a length of 50cm and a diameter of 3cm and dry-fill the activated silica gel with a negative pressure oscillating column filling device, vibrate up and down at a frequency of 70 times / min, and activate the silica gel at 105°C for 1.5h in an oven; Connect the negative pressure chromatography device, connect the developer device at the lower end, hang the developer container on the upper end of the column, create a height difference, carry out negative pressure upward development, the developer is chloroform:methanol=300:18, inject the bottom with a syringe Sample, the sample is a solution of 0.4g 70% vinorelbine crude product dissolved in 0.4ml developer; after spreading to the top of the column, cut the 10cm part 8cm from the bottom of the column, and ultrasonically elute it 3 times with 250ml absolute ethanol , 10 min each time, combined eluents; eluents were vacuum-filtered with a 0.22 μm hollow fiber, then concentrated under negative pres...

Embodiment 2

[0017] Take a hollow PVC column with a length of 45cm and a diameter of 3cm and dry-fill the activated silica gel with a negative pressure oscillating column filling device, add horizontal vibration up and down, and the frequency is 80 times / min. Connect the negative pressure chromatography device, connect the developer device at the lower end, hang the developer container on the upper end of the column, create a height difference, and perform negative pressure upward development, the developer is chloroform:methanol=250:18, and the bottom is used for automatic sampling Valve injection, the sample is a solution of 0.3g of 77% crude Vinorelbine dissolved in 0.3ml of developer; after reaching the top of the column, cut the part 4cm from the bottom of the column and 10cm upwards, and use 300ml of anhydrous methanol for ultrasonic elution 2 times, 20 minutes each time, combine the eluate; the eluate is filtered with a 0.22 μm hollow fiber under negative pressure, then concentrated ...

Embodiment 3

[0019] Take a hollow PVC column with a length of 55 cm and a diameter of 3 cm, and use a negative pressure oscillating column filling device to pour activated silica gel in the method, and vibrate up and down at a frequency of 90 times / min. The upper end of the silica gel column is connected to a negative pressure chromatography device, and the lower end is connected to a developing agent device. The developing agent container is at the same level as the silica gel column, and the developing agent is automatically sucked in through the negative pressure to perform negative pressure upward development. The developing agent is carbon tetrachloride: Methanol = 100:20, the bottom is injected with an automatic sampling valve, the sample is a solution of 0.5g of 70% vinorelbine crude product dissolved in 0.5ml of developing solvent; after spreading to the top of the column, cut upwards at 6cm from the bottom of the column The 12cm portion was stirred and eluted twice with 350ml of an...

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PUM

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Abstract

A process for purifying vinorelbine includes preparing silica gel column, negative-pressure chromatography by filling liquid from its bottom, segmental cutting, eluting, filtering, low-temp vacuum concentrating, dripping it in water to obtain crystals, centrifugal depositing, and drying the deposit.

Description

Technical field: [0001] The invention relates to a vinorelbine purification process. In particular, it relates to a method for purifying vinorelbine by means of negative pressure upward chromatography. Background technique: [0002] Vinorelbine is a drug approved by the U.S. Food and Drug Administration (FDA) for the treatment of patients with advanced non-small cell lung cancer (NSCLC). The combination of single-agent vinorelbine and cisplatin becomes unresectable advanced non-small cell lung cancer. The first-line treatment drug for patients is also the drug of choice in the treatment of breast cancer, lymphoma, and ovarian cancer, and its market price is expensive. At present, the market sources are mainly obtained through chemical synthesis, and the purity is not very high. To solve this problem, the present invention has found a purification method that can be used for large-scale production, so it has a good development prospect. [0003] In 1974, Vinorelbine was syn...

Claims

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Application Information

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IPC IPC(8): C07D519/04
Inventor 祖元刚付玉杰张琳史权刘君星李庆勇祖柏实曹玉杰
Owner NORTHEAST FORESTRY UNIVERSITY
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