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A method for HPLC analysis and separation of enantiomers of p-phenylbenzoylcorylide

A technology of phenylbenzoyl family and enantiomers, which is applied in the direction of material separation, analytical materials, scientific instruments, etc., can solve the problems affecting the quality of prostaglandin drugs, and the analysis and separation methods have not been reported, so as to ensure the The effect of quality controllability, ensuring stability, and good separation effect

Active Publication Date: 2018-09-11
CHANGCHUN BC&HC PHARMA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The two are enantiomers of each other, and the impurities continue to participate in the reaction in the subsequent steps to form a variety of corresponding impurities, which in turn affect the quality of prostaglandin drugs
However, there is no report on the separation method for the analysis and separation of the enantiomers of p-phenylbenzoylcoridone

Method used

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  • A method for HPLC analysis and separation of enantiomers of p-phenylbenzoylcorylide
  • A method for HPLC analysis and separation of enantiomers of p-phenylbenzoylcorylide
  • A method for HPLC analysis and separation of enantiomers of p-phenylbenzoylcorylide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Instruments and Conditions

[0023] Chromatographic column: BC chiral AD-H (250×4.6mm, 5.0μm)

[0024] Mobile phase: absolute ethanol

[0025] Column temperature: room temperature

[0026] Flow rate: 0.2mL / min

[0027] Injection volume: 1μL

[0028] Sample concentration: 10μg / mL

[0029] Detection wavelength: 275nm

[0030] Experimental procedure

[0031] Precisely measure 10 mg of (±)-p-phenylbenzoyl corilide, place it in a 10 mL volumetric flask, dissolve it in absolute ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Precisely draw 100 μL of the mother solution of the test product, place it in a 10 mL volumetric flask, dilute it to the mark with absolute ethanol, and prepare a solution of the test product with a concentration of 10 μg / mL. Take (±)-p-phenylbenzoyl corilide test solution 1μL into the liquid chromatography, record the chromatogram.

[0032] Experimental results: the separation degree of the two en...

Embodiment 2

[0034] Instruments and Conditions

[0035] Chromatographic column: BC chiral AD-H (250×4.6mm, 5.0μm)

[0036] Mobile phase: absolute ethanol

[0037] Column temperature: room temperature

[0038] Flow rate: 0.3mL / min

[0039] Injection volume: 5μL

[0040] Sample concentration: 5μg / mL

[0041] Detection wavelength: 280nm

[0042] Experimental procedure

[0043] Precisely measure 10 mg of (±)-p-phenylbenzoyl corilide, place it in a 10 mL volumetric flask, dissolve it in absolute ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Precisely draw 50 μL of the mother solution of the test product, place it in a 10 mL volumetric flask, dilute it to the mark with absolute ethanol, and prepare a solution of the test product with a concentration of 5 μg / mL. Take (±)-p-phenylbenzoyl corilide 5 μL of the test solution into the liquid chromatograph, and record the chromatogram.

[0044] Experimental results: the separation degree of th...

Embodiment 3

[0046] Instruments and Conditions

[0047] Chromatographic column: BC chiral AD-H (250×4.6mm, 5.0μm)

[0048] Mobile phase: absolute ethanol

[0049] Column temperature: room temperature

[0050] Flow rate: 0.4mL / min

[0051] Injection volume: 10μL

[0052] Sample concentration: 1μg / mL

[0053] Detection wavelength: 280nm

[0054] Experimental procedure

[0055] Precisely measure 10 mg of (±)-p-phenylbenzoylcoridone body, place it in a 10 mL volumetric flask, dissolve it in absolute ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Precisely draw 10 μL of the mother solution of the test product, place it in a 10 mL volumetric flask, dilute it to the mark with absolute ethanol, and prepare a solution of the test product with a concentration of 1 μg / mL. Take (±)-p-phenylbenzoyl corilide test solution 10 μ L into the liquid chromatography, record the chromatogram.

[0056] Experimental results: see attachedfigure 1 , (+)-p-p...

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Abstract

The invention discloses a method for HPLC analysis and separation of 4-phenylbenzoyl Corey lactone enantiomers; a chiral chromatographic column is adopted for analysis, separation and determination by normal phase chromatography. The method can simply, accurately and efficiently analyze and separate the 4-phenylbenzoyl Corey lactone enantiomers, so as to achieve quality control of the 4-phenylbenzoyl Corey lactone enantiomers. The method can also be used for preparation of high-purity single-opticity 4-phenylbenzoyl Corey lactone.

Description

technical field [0001] The invention relates to a chromatographic analysis and separation method, in particular to a high-performance liquid chromatography method for analyzing and separating the enantiomers of p-phenylbenzoylcorilelide. technical background [0002] Prostaglandins (PGs for short) are a class of important substances with endogenous physiological activities, which widely exist in various tissues in the body and are important mediators of various physiological processes. Due to the extremely low content in the human body, prostaglandin drugs are mainly synthesized clinically. Corey lactonephenylbenzoate is a commonly used intermediate and starting material for the synthesis of prostaglandin drugs, and its molecular formula is C 21 h 20 o 5 , chemical name: hexahydro-4-(hydroxymethyl)-2-oxo-2H-cyclopenta[b]furan-5-yl 1,1'-biphenyl-4-carboxylate, common name It is: p-phenylbenzoyl corilide, the structural formula is: [0003] [0004] There are 4 chiral ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/065
Inventor 修志明王淑红李黎赵春影范修康李春英
Owner CHANGCHUN BC&HC PHARMA TECH CO LTD
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