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A method for detecting milobalin and its enantiomer impurities by high performance liquid chromatography

A high-performance liquid chromatography and enantiomer technology, applied in the field of pharmaceutical analysis, can solve the problems of weak ultraviolet absorption, limited normal-phase method development, large polarity, etc., and achieve the effects of good durability and good injection repeatability.

Active Publication Date: 2022-02-11
NANJING VCARE PHARMATECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The raw material of milobarin exists in the form of besylate, and there are fewer double bonds in the structural formula, and the ultraviolet absorption is weaker; the compound has obvious acidic and basic groups, and the polarity is larger; the compound has a chiral center, There is also cis-trans isomerism, and the separation of enantiomers is poor, which is subject to many restrictions in the development of normal phase methods. At present, there are no literature reports on the separation and detection methods of milobalin and its enantiomer impurities.

Method used

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  • A method for detecting milobalin and its enantiomer impurities by high performance liquid chromatography
  • A method for detecting milobalin and its enantiomer impurities by high performance liquid chromatography
  • A method for detecting milobalin and its enantiomer impurities by high performance liquid chromatography

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Effect test

Embodiment 1

[0024] Embodiment 1: Screening of chromatographic conditions

[0025] Screen and determine the chromatographic conditions through chromatographic column, mobile phase, wavelength, flow rate, etc.

Embodiment 1-a

[0027] Chromatographic column: Daicel ADH 250×4.6mm, 5um;

[0028] Detection wavelength: 265 nm; column temperature: 25 ℃; injection volume: 10 uL; flow rate: 0.5 mL / min;

[0029] The mobile phase is n-hexane:ethanol=90:10, and the elution is isocratic according to 0 min and 60 min;

[0030] Conclusion: Using neutral system and Daicel ADH column, the peak elutes earlier and the peak shape is poor.

Embodiment 1-b

[0032] Try adding trifluoroacetic acid and diethylamine to the mobile phase on the basis of Example 1-a;

[0033] Chromatographic column: Daicel ADH 250×4.6mm, 5um;

[0034] Detection wavelength: 265 nm; column temperature: 25 ℃; injection volume: 10 uL; flow rate: 0.5 mL / min;

[0035] The mobile phase is n-hexane: ethanol: trifluoroacetic acid: diethylamine=90: 10: 0.05: 0.1;

[0036] According to 0 min, 60min isocratic elution;

[0037] Conclusion: Adding trifluoroacetic acid and diethylamine to the mobile phase on the basis of Example 1-a, the main component and enantiomers of milopalin came out earlier, and the peak shape was slightly improved, but they were not separated.

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Abstract

The invention relates to a method for detecting milobalin and its enantiomer impurities by high-performance liquid chromatography. The chromatographic column CHIRAL-AGP of the method uses α1-acid glycoprotein bonded silica gel as a filler; the concentration is 5-30 mMol Ammonium acetate buffer solution-isopropanol / L is the mobile phase, the ratio is 97-99:3-1; the detection wavelength is 200 nm-210 nm; the column temperature is 20-25°C; the flow rate of the mobile phase is 0.2-0.5 mL / min; the method for detecting milobalin and its enantiomer impurities by high performance liquid chromatography provided by the invention can realize the separation degree of milobalin main component and its enantiomer impurities R ≥ 1.8, continuous sample injection of the test solution The impurity content of 6 enantiomers was RSD≤0.1%, the injection repeatability was good, and the method had good durability, which could be used for the quality control of milopalin.

Description

technical field [0001] The invention belongs to the field of drug analysis, and in particular relates to a method for detecting milopalin and its enantiomer impurities by high performance liquid chromatography. Background technique [0002] Mirogabalin (DS-5565) is a drug developed by Daiichi Pharmaceutical Sankyo Co., Ltd., which is similar to drugs such as gabapentin and pregabalin. Milobalin is a novel preferentially selective α2δ-1 ligand with high potency and selectivity for the α2δ-1 subunit of voltage-sensitive calcium channel complexes in the central nervous system (CNS). Milogabalin binds to α2δ calcium channels (1 and 2), but with significantly higher potency than pregabalin. Promising results have been shown in phase II clinical trials for the treatment of diabetic peripheral neuropathic pain. Its structural formula is as follows: [0003] . [0004] The raw material of milobarin exists in the form of besylate, and there are fewer double bonds in the structu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 嵇俊晔梁兆娟周西朋刘永强龚彦春杨尚彦
Owner NANJING VCARE PHARMATECH CO LTD
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