Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for analyzing and preparing diacetyl corey lactone enantiomer by HPLC method

A technology of enantiomers and corylides, which is applied in the field of chemical raw material preparation, can solve the problems such as few reports of enantiomers of diacetyl corylides, so as to ensure quality, good separation effect, and ensure The effect of stability

Active Publication Date: 2018-12-07
JINLIN MEDICAL COLLEGE
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In recent years, with the diversification of chiral chromatographic packing materials, the application of chiral chromatographic column liquid chromatography has become more and more extensive. However, the use of chiral chromatographic column high performance liquid There are reports

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for analyzing and preparing diacetyl corey lactone enantiomer by HPLC method
  • Method for analyzing and preparing diacetyl corey lactone enantiomer by HPLC method
  • Method for analyzing and preparing diacetyl corey lactone enantiomer by HPLC method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: the analysis of (-)-diacetyl corilide and (+)-diacetyl corilide

[0043] Instruments and Conditions

[0044] Column: AD-H (250×4.6mm, 5.0μm)

[0045] Mobile phase: n-hexane-ethanol (95:5)

[0046] Column temperature: 40°C

[0047] Flow rate: 1.0mL / min

[0048] Injection volume: 5μL

[0049] Sample concentration: 1mg / mL

[0050] Detection wavelength: 205nm

[0051] Experimental procedure

[0052] Accurately measure 1 mg each of (+)-diacetylcorylide and (-)-bisacetylcorylide respectively, place in a 10mL volumetric flask, dissolve in ethanol and dilute to the mark, shake well, and use it as a reference solution. Accurately weigh 10 mg of (±)-diacetylcorylide, place it in a 10 mL volumetric flask, dissolve it in ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Accurately draw 5 μL each of the reference substance and the mother solution of the test product into the liquid chromatogram, and refer to the...

Embodiment 2

[0054] Embodiment 2: the analysis of (-)-diacetyl corilide and (+)-diacetyl corilide

[0055] Instruments and Conditions

[0056] Column: AD-H (250×4.6mm, 5.0μm)

[0057] Mobile phase: n-hexane-ethanol (60:40)

[0058] Column temperature: 20°C

[0059] Flow rate: 0.5mL / min

[0060] Injection volume: 10μL

[0061] Sample concentration: 0.1mg / mL

[0062] Detection wavelength: 205nm

[0063] Experimental procedure

[0064] Accurately measure 1 mg each of (+)-diacetylcorylide and (-)-bisacetylcorylide respectively, place in a 10mL volumetric flask, dissolve in ethanol and dilute to the mark, shake well, and use it as a reference solution. Accurately weigh 10 mg of (±)-diacetylcorylide, place it in a 10 mL volumetric flask, dissolve it in ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Precisely draw 1mL of the mother solution of the test product, place it in a 10mL volumetric flask, dissolve it in ethanol and dilute to th...

Embodiment 3

[0066] Embodiment 3: the analysis of (-)-diacetyl corilide and (+)-diacetyl corilide

[0067] Instruments and Conditions

[0068] Column: AD-H (250×4.6mm, 5.0μm)

[0069] Mobile phase: n-hexane-ethanol (75:25)

[0070] Column temperature: 30°C

[0071] Flow rate: 0.8mL / min

[0072] Injection volume: 5μL

[0073] Sample concentration: 1mg / mL

[0074] Detection wavelength: 205nm

[0075] Experimental procedure

[0076] Accurately measure 1 mg each of (+)-diacetylcorylide and (-)-bisacetylcorylide respectively, place in a 10mL volumetric flask, dissolve in ethanol and dilute to the mark, shake well, and use it as a reference solution. Accurately weigh 10 mg of (±)-diacetylcorylide, place it in a 10 mL volumetric flask, dissolve it in ethanol and dilute to the mark, shake well, and use it as the mother solution of the test sample. Accurately draw 5 μL each of the reference substance and the mother solution of the test product into the liquid chromatogram, and refer to th...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Wavelengthaaaaaaaaaa
Login to View More

Abstract

The present invention discloses a method for analyzing and preparing a diacetyl corey lactone enantiomer by a HPLC method, a polysaccharide derivative-coated chiral HPLC column is used as a stationaryphase, a n-hexane-isopropanol mixed solvent or a n-hexane-ethanol mixed solvent is used as a mobile phase, and a normal phase chromatography method is used for analysis and separation. The method issimple, accurate and efficient for analysis and preparation of the diacetyl corey lactone enantiomer with single optical activity, thus achieving the quality control of the diacetyl corey lactone enantiomer.

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 preparing diacetylcorylide enantiomers, and belongs to the technical field of chemical raw material preparation. Background technique [0002] Prostaglandins are an important class of endogenous physiologically active substances, which regulate various physiological functions of the human body at the level of hormone concentration, and have regulatory effects on blood pressure, smooth muscle contraction, gastric juice secretion and platelet aggregation. Prostaglandins are trace components that widely exist in human and animal tissues, and the content is extremely low. Clinically, prostaglandin drugs are mainly produced by total synthesis. [0003] Diacetylcorylide is an important intermediate in the synthesis of prostaglandins, and its chemical name is: 6-acetoxymethyl-7-acetoxy-cis-2-oxabicyclo[3...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 修志明王淑红李志波王丽萍刘莉
Owner JINLIN MEDICAL COLLEGE