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Method for separating milobalin intermediate and enantiomer thereof by high performance liquid chromatography

A high-performance liquid chromatography and enantiomer technology, which is applied in the field of high-performance liquid chromatography for separating milobaline intermediates and their enantiomers, and can solve the problems of cumbersome processing, low safety, problems such as low sensitivity, to achieve the effect of good injection repeatability, high safety and high sensitivity

Pending Publication Date: 2022-04-01
JIANGSU VCARE PHARMATECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The problem to be solved by the present invention is that the prior art has low sensitivity, high cost, cumbersome and low safety in the separation of milopalin intermediates and their enantiomers, and the central control detection sample processing

Method used

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  • Method for separating milobalin intermediate and enantiomer thereof by high performance liquid chromatography
  • Method for separating milobalin intermediate and enantiomer thereof by high performance liquid chromatography
  • Method for separating milobalin intermediate and enantiomer thereof by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Screening of Chromatography (Positive Phase)

[0035] The chromatographic conditions were determined by column, mobile phase, wavelength, flow rate, and the like.

Embodiment 1-a

[0037] Column: AD-H column 250mm × 4.6mm, 5 μm;

[0038] Test wavelength: 210 nm; column temperature: 30 ° C; injection volume: 10 μL; flow rate: 0.5 mL / min;

[0039] The flow phase is n-hexane: ethanol = 80:20, eluting according to 0 min, 40 min et al.;

[0040] Conclusion: AD-H pillar, Milo Bahrain intermediate and its enantiomer peak peaks are premature, and the separation is poor.

Embodiment 1-b

[0042] Attempts to adjust the flow phase and the column temperature on the basis of Example 1-A;

[0043] Column: The AD-H column 250mm × 4.6mm, 5 μm;

[0044] Detection wavelength: 210 nm; column temperature: 25 ° C; injection volume: 10 μL; flow rate: 0.5 mL / min;

[0045] The flow phase is n-hexane: isopropanol = 98: 2, eluting according to 0 min, 45 min is equal;

[0046] Conclusion: AD-H column is used to change the mobile phase and its ratio. After adjusting the column temperature, the Milo Bahrain Intermediate and its enantioma separation are slightly improved, but it has not yet reached the baseline separation requirements.

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Abstract

The invention relates to a method for separating a milobain intermediate and an enantiomer thereof by high performance liquid chromatography, which is characterized in that a chromatographic column adopts a polysaccharide derivative reverse-phase coating type chiral chromatographic column, and the surface of silica gel is coated with cellulose-tri (3, 5-dimethyl phenyl carbamate); phosphoric acid aqueous solution-acetonitrile with the concentration of 0.02-0.10% is adopted as a mobile phase, and the ratio of the phosphoric acid aqueous solution to the acetonitrile is (55-70): (45-30); the detection wavelength is 205 nm to 215 nm; the column temperature is 15-30 DEG C; the flow velocity of the mobile phase is 0.3-1.0 mL / min; the high performance liquid chromatography provided by the invention can realize complete separation of the milobabalin intermediate and the enantiomer thereof, has good sample introduction repeatability and good durability, and can be used for quality control of the milobabalin intermediate.

Description

Technical field [0001] The present invention belongs to the field of drug analysis, and more particularly to a method of separating Milo Bahrain intermediates and enantiomers thereof in high performance liquid chromatography. Background technique [0002] Mirogabalin (DS-5565) is a drug developed by the First Pharmaceutical Trinity Co., Ltd., similar to drugs such as Gabobalin. Milobalin is a new priority selective α2δ-1 ligand, which has efficient and selective α2δ-1 subunits of the voltage-sensitive calcium channel complex in the central nervous system (CNS). Milobalin binds to α2δ calcium channels (1 and 2), but the performance is significantly higher than that in Puababalin. A good effect is shown in the II clinical trial of the treatment of neurological pain around diabetes. [0003] [0004] (1R, 5S) -3-ethyl bicyclic [3.2.0] hept-3-u-6-ketone is a Milo Bahrain intermediate, its enantiomer is (1S, 5R) -3-ethyl Benx [3.2.0] hept-3-olene-6-ketone, the two-bonds in the struc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 嵇俊晔丁文涛梁兆娟周西朋刘永强龚彦春杨尚彦
Owner JIANGSU VCARE PHARMATECH
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