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Method for preparing lonicerae flos monomer with dynamic axial compression column

A technology of axial compression and honeysuckle, applied in the field of biochemistry, can solve the problems of cumbersome separation steps, low purity of chlorogenic acid, large solvent consumption, etc., and achieve simple preparation process, high utilization rate of plant resources, and short production cycle Effect

Active Publication Date: 2017-01-11
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the purity of chlorogenic acid obtained by the industrial method of preparing chlorogenic acid is relatively low, and high-purity chlorogenic acid can only be obtained through multi-step separation and purification, and the preparation process is complicated, the separation steps are cumbersome, and the solvent consumption is large

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  • Method for preparing lonicerae flos monomer with dynamic axial compression column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 50g of honeysuckle medicinal materials, add 60% ethanol, and ultrasonically extract for 30 minutes; filter the extract and remove the filter residue, and concentrate the filtrate to a clear paste with a density of 1.02-1.05; extract once with 3 times the amount of ethyl acetate, and extract Concentrate to dryness; dilute the ethyl acetate extract with mobile phase to a concentration of 42mg / ml as the sample solution; add 1000g of C18 filler with a particle size of 10μm, add 2800mL homogenization reagent, set the DAC column system pressure, at room temperature After sonicating for 30 minutes, sonicating and stirring for 20 minutes, send the homogenate into a dynamic axial compression column with a diameter of 80mm, and compact the column packing after removing the mobile phase to complete the packing of the DAC column; use the mobile phase to continuously flush the dynamic axial compression Column 15-20 minutes until the baseline of the chromatograph is stable; set t...

Embodiment 2

[0032] Weigh 50g of honeysuckle medicinal materials, add 60% ethanol, and extract at reflux for 30min; filter the extract and remove the filter residue, concentrate the filtrate to a clear paste with a density of 1.02-1.05; extract once with 3 times the amount of ethyl acetate, the extract Concentrate to dryness; dilute the ethyl acetate extract with mobile phase to a concentration of 42mg / ml as the sample solution; add 1000g of C18 filler with a particle size of 10μm, add 2800mL homogenization reagent, set the DAC column system pressure, at room temperature After sonicating for 30 minutes, sonicating and stirring for 20 minutes, send the homogenate into a dynamic axial compression column with a diameter of 80mm, and compact the column packing after removing the mobile phase to complete the packing of the DAC column; use the mobile phase to continuously flush the dynamic axial compression Column 15-20 minutes until the baseline of the chromatograph is stable; set the wavelength ...

Embodiment 3

[0034] Weigh 50g of honeysuckle medicinal materials, add 60% ethanol, and microwave extraction for 30min; filter the extract and remove the filter residue, concentrate the filtrate to a clear paste with a density of 1.02-1.05; extract once with 3 times the amount of ethyl acetate, the extract Concentrate to dryness; dilute the ethyl acetate extract with mobile phase to a concentration of 42mg / ml as the sample solution; add 1000g of C18 filler with a particle size of 10μm, add 2800mL homogenization reagent, set the DAC column system pressure, at room temperature After sonicating for 30 minutes, sonicating and stirring for 20 minutes, send the homogenate into a dynamic axial compression column with a diameter of 80mm, and compact the column packing after removing the mobile phase to complete the packing of the DAC column; use the mobile phase to continuously flush the dynamic axial compression Column 15-20 minutes until the baseline of the chromatograph is stable; set the waveleng...

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Abstract

The invention relates to the technical field of medicine, and discloses a method for separating and purifying the four monomers neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid and secoxyloganin from lonicerae flos with a dynamic axial compression column. The method comprises the steps of mobile phase preparation, dissolution and filtration, dynamic axial compression column packing, system balancing, elution and separation, concentration and the like. With the method, the four monomers neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid and secoxyloganin can be prepared at a same time in one separation purification process. As a result of high performance liquid chromatography detection, the purities of the four monomers are all above 90%. The method provided by the invention has the advantages of simple operation, short production period, high preparation efficiency, and controllable product quality. All adopted organic reagents can be recycled. The method is a highly efficient, environment-friendly and highly applicable separation purification method for industrial preparation of lonicerae flos monomers.

Description

Technical field [0001] The invention relates to the field of biochemistry, in particular to a method for preparing honeysuckle monomers by using a dynamic axial compression column. Background technique [0002] Honeysuckle (Lonicerae Flos) is the dried flower buds or first-opening flowers of Lonicera japonica Thunb., a plant of the family Caprifoliaceae. It has the effects of clearing away heat, detoxifying, and dispersing wind heat. Used for carbuncle swelling and furuncle, throat numbness, erysipelas, heat toxin blood dysentery, wind-heat cold, febrile fever and fever. [0003] The main components of honeysuckle are organic acids, volatile oils, flavonoids, triterpene saponins, and inorganic elements. Chlorogenic acid compounds are the main active ingredients of honeysuckle. The main pharmacological effects of honeysuckle are: 1. Antibacterial and antiviral effects. Honeysuckle has a certain inhibitory effect on a variety of pathogenic bacteria, including Staphylococcus aureu...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08C07C69/732C07C67/48C07C67/56
CPCY02P20/582
Inventor 殷军韩娜刘志惠李陆晖
Owner SHENYANG PHARMA UNIVERSITY
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