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Method for analytical separation of (-) benzoyl Corey lactone optical isomers by HPLC

A technology of optical isomers and benzoyl family, which is applied in the field of high performance liquid chromatography, can solve the problem of no benzoyl corilide and other problems, achieve good analysis and separation effect, ensure quality control, and improve symmetry sexual effect

Active Publication Date: 2015-04-22
WUHAN WUYAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The separation of optical isomers containing chiral carbon atoms has always been a difficult point in quality control during the synthesis and preparation of chiral drugs. After searching the literature, there is no detection method for (-) benzoylcorilide optical isomers. to report

Method used

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  • Method for analytical separation of (-) benzoyl Corey lactone optical isomers by HPLC
  • Method for analytical separation of (-) benzoyl Corey lactone optical isomers by HPLC
  • Method for analytical separation of (-) benzoyl Corey lactone optical isomers by HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Instruments and Conditions

[0032] Chromatographic column: AD-H (Daicel, 250mm×4.6mm, 5μm);

[0033] Mobile phase: n-hexane-absolute ethanol=89:11;

[0034] Column temperature: 40°C;

[0035] Flow rate: 1.0ml / min;

[0036] Injection volume: 20μl;

[0037] Detection wavelength: 220nm;

[0038] Experimental procedure

[0039] Weigh 10 mg each of (-) benzoylcorilide and its optical isomer, put it in a 10 ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and use it as a system suitability solution. Take (-) 10mg of benzoylcolide, accurately weighed, put it in a 10ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and use it as the test solution. Take (+) 10mg of benzoylcolide, accurately weigh it, put it in a 10ml measuring bottle, dissolve it with absolute ethanol and dilute to the mark, shake well, take 1ml precisely, put it in a 100ml measuring bottle, and use anhydrous Dilute with eth...

Embodiment 2

[0042] Instruments and Conditions

[0043] Chromatographic column: AD-H (Daicel, 250mm×4.6mm, 5μm);

[0044] Mobile phase: n-hexane-absolute ethanol=92:8;

[0045] Column temperature: 35°C;

[0046] Flow rate: 1.0ml / min;

[0047] Injection volume: 20μl;

[0048] Detection wavelength: 220nm;

[0049] Experimental procedure

[0050] Weigh 10 mg each of (-) benzoylcorilide and its optical isomer, put it in a 10 ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and use it as a system suitability solution. Take (-) 10mg of benzoylcolide, accurately weighed, put it in a 10ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and use it as the test solution. Take (+) 10mg of benzoylcolide, accurately weigh it, put it in a 10ml measuring bottle, dissolve it with absolute ethanol and dilute to the mark, shake well, take 1ml precisely, put it in a 100ml measuring bottle, and use anhydrous Dilute with etha...

Embodiment 3

[0053] Instruments and Conditions

[0054] Chromatographic column: AD-H (Daicel, 250mm×4.6mm, 5μm);

[0055] Mobile phase: n-hexane-absolute ethanol=92:8;

[0056] Column temperature: 40°C;

[0057] Flow rate: 1.0ml / min;

[0058] Injection volume: 20μl;

[0059] Detection wavelength: 220nm;

[0060] Experimental procedure

[0061]Weigh 10 mg each of (-) benzoylcorilide and its optical isomer, put it in a 10 ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and use it as a system suitability solution. Take (-) 10mg of benzoylcolide, accurately weighed, put it in a 10ml measuring bottle, add absolute ethanol to dissolve and dilute to the mark, shake well, and use it as the test solution. Take (+) benzoylcolide 10mg, accurately weigh it, put it in a 10ml measuring bottle, dissolve it with absolute ethanol and dilute to the mark, shake well, accurately measure 1ml, put it in a 100ml measuring bottle, and use anhydrous Dilute with etha...

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Abstract

The invention discloses an analysis and separation determination method for (-) benzoyl Corey lactone and its optical isomers by high performance liquid chromatography (HPLC). A cellulose chiral column is adopted, and a normal phase mixed solvent is taken as a mobile phase to perform separation by normal-phase chromatography. With the method, (-) benzoyl Corey lactone and its optical isomer impurities can be rapidly separated.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography, in particular to a high-performance liquid chromatography for analyzing and separating (-) benzoyl corilide and its optical isomers. Background technique [0002] (-) Benzoyl corilide is a commonly used intermediate or starting material for the synthesis of prostaglandin drugs, and its molecular formula is C 15 h 16 o 5 , the chemical name is (3aR,4S,5R,6aS)-(-)-5-(benzoyloxy)-hexahydro-4-(hydroxymethyl)-2H-cyclopenta[b]furan-2 - Ketone, the structural formula is [0003] [0004] The molecule contains 4 chiral centers, and theoretically there are multiple optical isomers, but combined with its synthesis method and reaction mechanism analysis, there is only one optical isomer that is most likely to exist, that is (+) benzoyl group Rilactone, this impurity can remain in prostaglandin drugs through subsequent reactions, affecting the quality of drugs. Therefore, controlling the co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60G01N30/06G01N30/02
Inventor 沈婕乔春莲杨波罗岩
Owner WUHAN WUYAO SCI & TECH
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