Method for separating and purifying cisatracurium besylate by preparative liquid chromatography

A kind of technology of atracurium besylate and atracurium besylate, applied in the field of medicinal chemistry, can solve problems such as no indication of industrialized production, manual operation, low yield, etc., achieve automatic operation, organic solvent The effect of less and higher yield

Inactive Publication Date: 2009-07-08
SHANGHAI PHARMA DONGYING JIANGSU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing references applied to the analytical chromatography of atracurium cis-benzenesulfonate do not show that it can be used for industrial production under existing known conditions, and most of these methods have low yield, large pollution, manual Operation and other disadvantages

Method used

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  • Method for separating and purifying cisatracurium besylate by preparative liquid chromatography

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Experimental program
Comparison scheme
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Embodiment 1

[0030] Equipment: Varian SD-1preparative HPLC

[0031] Chromatographic column: spherical silica gel, 16um, 250mm×110mmID

[0032] Mobile phase: A dichloromethane; B methanol = 100:10, adjust the pH value to 3-4 with benzenesulfonic acid

[0033] Duty ratio: 150

[0034]Column pressure: 300psi

[0035] Column temperature: 5-10°C

[0036] Flow rate: 300ml / min

[0037] Detection wavelength: 280nm

[0038] Injection volume: 10g / injection

[0039] After dissolving the crude product of atracurium besylate obtained by synthesis with a mobile phase, load it on a chromatographic column, then elution and separation with a mobile phase, collect in sections to obtain a cisatracurium solution, wash with 10% saline, and organic The layers were concentrated and dried under reduced pressure, the concentrated solution was dissolved in water, adjusted to pH=4.0 with benzenesulfonic acid, and freeze-dried to obtain an off-white or off-white solid—atracurium cis-benzenesulfonate, with a pro...

Embodiment 2

[0041] The stationary phase was adjusted to 10 micron spherical silica gel, the mobile phase was adjusted to dichloromethane:methanol=100:20, and the load ratio was 100. Others were the same as in Example 1. The yield of the final product was 80%, and the purity was greater than 96%.

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Abstract

The invention discloses a method for separating and purifying cis-benzene sulfonic acid atracurium through preparative liquid chromatography, which is to use a mobile phase to dissolve benzene sulfonic acid atracurium, load the benzene sulfonic acid atracurium on a preparative liquid-phase chromatographic silica gel column, perform normal-phase or opposite-phase liquid-phase chromatographic separation under the elution of the mobile phase, and reclaim the cis-benzene sulfonic acid atracuriums, wherein immobile-phase silica gel is modified bonded silica gel, and the particle diameter of the immobile-phase silica gel is between 1 and 200 micrometers; the load ratio of the immobile-phase silica gel to atracurium is not more than 1,000; and the pressure of the silica gel column is between 250 and 400 psi. The cis-benzene sulfonic acid atracurium obtained by the method has high purity, high yield and low cost; the amount of an organic solvent used is low; the pollution is light; and the maneuverability is strong. The treatment time of the method is shortened by approximately 10 times compared with the prior art, and simultaneously the method can feed samples continuously, realize automatic operation and the like.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a method for separating and purifying atracurium cis-benzenesulfonate through preparation liquid chromatography. Background technique [0002] Atracurium besylate is a classic non-depolarizing muscle relaxant with moderate time effect, which is widely used in clinical anesthesia. Cisatracurium besylate is a single isomer of atracurium besylate, which has similar muscle relaxant effect and metabolic mode as atracurium besylate, but its muscle relaxant strength is about It is 3 times that of the drug, does not release histamine, and has a small cardiovascular response. It is an ideal non-depolarizing muscle relaxant with a medium-term effect. [0003] The structural formula of cis-atracurium besylate is as follows: [0004] [0005] The structure of atracurium besylate is relatively complex. The molecule contains 4 chiral centers, 2 of which are chiral carbon and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D217/20B01D15/08B01D15/42
Inventor 黄乐群王磊贺乾辉
Owner SHANGHAI PHARMA DONGYING JIANGSU PHARMA CO LTD
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