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Method for analyzing and separating Corey lactone benzoate enantiomers through HPLC

An enantiomer, benzoylide technology, applied in the field of analysis and separation of benzoylcolide enantiomers by high performance liquid chromatography, can solve the problem of low stereoselectivity and relatively poor interaction differences. Small, enantiomers cannot be effectively separated, etc., to achieve the effect of high stereoselectivity, improve symmetry, and ensure quality controllability

Active Publication Date: 2016-09-21
吉林百纯化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there are few studies on the analysis and separation methods of benzoylcorylide enantiomers in the prior art, and there are some problems and deficiencies in the only exploratory studies, such as the amylose-amylose-coated silica gel surface in the chromatographic column. Tris-(3,5-dimethylphenylcarbamate) filler has less difference in interaction with benzoylcorylide enantiomers and lower stereoselectivity, making benzoylcorylide Lactone enantiomers cannot be separated efficiently

Method used

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  • Method for analyzing and separating Corey lactone benzoate enantiomers through HPLC
  • Method for analyzing and separating Corey lactone benzoate enantiomers through HPLC
  • Method for analyzing and separating Corey lactone benzoate enantiomers through HPLC

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Instruments and Conditions

[0030] Chromatographic column: Daicel AD-H (250×4.6mm, 5.0μm)

[0031] Mobile phase: n-hexane-absolute ethanol (90:10)

[0032] Column temperature: 30°C

[0033] Flow rate: 1.0mL / min

[0034] Sample concentration: 10μg / mL

[0035] Injection volume: 2μL

[0036] Detection wavelength: 220nm

[0037] Experimental procedure

[0038] Accurately weigh (±)-benzoyl corilide 10mg, place in a 10mL volumetric flask, dissolve and dilute to the mark with n-hexane-isopropanol (90:10), 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 and place it in a 10mL volumetric flask, adjust the volume of n-hexane-isopropanol (90:10) solution to the mark, and prepare (±)-benzoylcoridone with a concentration of 10 μg / mL Need testing solution, draw need testing solution 2 μ L and enter liquid chromatography, record chromatogram.

[0039] Experimental results: see attached figure ...

Embodiment 2

[0041] Instruments and Conditions

[0042] Chromatographic column: BC chiral AS-H (250×4.6mm, 5.0μm)

[0043] Mobile phase: n-hexane-isopropanol (90:10)

[0044] Column temperature: room temperature

[0045] Flow rate: 1.0mL / min

[0046] Sample concentration: 10μg / mL

[0047] Injection volume: 1μL

[0048] Detection wavelength: 210nm

[0049] Experimental procedure

[0050]Accurately weigh (±)-benzoyl corilide 10mg, place in a 10mL volumetric flask, dissolve and dilute to the mark with n-hexane-isopropanol (90:10), 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 and place it in a 10mL volumetric flask, adjust the volume of n-hexane-isopropanol (90:10) solution to the mark, and prepare (±)-benzoylcoridone with a concentration of 10 μg / mL For the test solution, draw 1 μL of the test solution into the liquid chromatograph, and record the chromatogram.

[0051] Experimental results: the sepa...

Embodiment 3

[0053] Instruments and Conditions

[0054] Chromatographic column: BC chiral AS-H (250×4.6mm, 5.0μm)

[0055] Mobile phase: n-hexane-isopropanol (80:20)

[0056] Column temperature: room temperature

[0057] Flow rate: 0.8mL / min

[0058] Sample concentration: 5μg / mL

[0059] Injection volume: 5μL

[0060] Detection wavelength: 235nm

[0061] Experimental procedure

[0062] Accurately weigh (±)-benzoyl corilide 10mg, place in a 10mL volumetric flask, dissolve and dilute to the mark with n-hexane-isopropanol (80:20), shake well, and use it as the mother solution of the test sample. Precisely draw 50 μL of the mother liquor and place it in a 10mL volumetric flask, adjust the volume to the mark with the n-hexane-isopropanol (80:20) solution, and prepare (±)-benzoylcoridone test sample with a concentration of 5 μg / mL solution, absorb 5 μL of the test solution into the liquid chromatograph, and record the chromatogram.

[0063] Experimental results: the separation degree of ...

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Abstract

The invention discloses a method for analyzing and separating Corey lactone benzoate enantiomers through an HPLC by means of a direct-chain starch type chiral chromatographic column with positive phase mixed solvent as the flowing phase. The method can easily, accurately and efficiently analyze and separate the Corey lactone benzoate enantiomers, and therefore the quality of the Corey lactone benzoate enantiomers is controlled. The method can also be used for preparing high-purity single-optical-activity Corey lactone benzoate.

Description

technical field [0001] The invention relates to a chromatographic analysis and separation method, in particular to a method for analyzing and separating the enantiomers of benzoylcoriletone by high-performance liquid chromatography. 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. Benzoyl cori lactone (Corey lactone benzoate) is a common starting material for the synthesis of prostaglandin drugs, and its molecular formula is C 15 h 16 o 5 , chemical name: 5-(benzoyloxy)hexahydro-4-(hydroxymethyl)-2H-cyclopenta[b]furan-2-one, common name: benzoylcorylide , the structural formula is: [0003] [0004] The molecule contains four chiral centers, and theoretically th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N30/60G01N2030/027
Inventor 王淑红李黎彭悦李宇珈李志波修志明
Owner 吉林百纯化学科技有限公司
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