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Method for purifying ceylon leucas herb ketone by using high-performance countercurrent chromatography

A high-efficiency countercurrent chromatography and cellulone technology, which is applied in the field of natural product separation, can solve problems such as no patents, and achieve the effects of avoiding sample loss, good product purity, and overcoming cumbersome operations

Inactive Publication Date: 2014-10-01
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no report on the separation and purification of total flavonoids of honeycomb grass by high-efficiency countercurrent chromatography, and there are no related patents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 1 kg of dried honeycomb grass, crush it, pass through a 40-mesh sieve, add 8 kg of 80% ethanol for ultrasonic extraction for 30 minutes, extract twice, the ultrasonic frequency is 40KHZ, add 1% activated carbon to the solution for decolorization, and filter. The filtrate is filtered through 1000D hollow fiber polysulfone membrane for impurity removal successively, the inlet pressure is 0.1MPa, and the 200D hollow fiber polysulfone membrane is concentrated by nanofiltration, the inlet pressure is 1.0MPa, and placed for crystallization.

[0020] Mix ethyl acetate-ethanol-water according to the volume ratio of 2:5:3, shake evenly by ultrasonic, stand and separate after layering, the lower phase is the solid phase, the upper phase is the mobile phase, the crystal is dissolved in the upper phase, and the stationary phase Pump the chromatographic column fully, then adjust the speed of the main engine to 800rmp, and then pump the mobile phase at a flow rate of 3ml / min. Aft...

Embodiment 2

[0022] Take 3 kg of dried honeycomb grass, crush it, pass through a 40-mesh sieve, add 30 kg of 80% ethanol for ultrasonic extraction for 60 minutes, extract 3 times, the ultrasonic frequency is 65KHZ, add 3% activated carbon to the solution for decolorization, and filter. The filtrate is successively passed through 3000D hollow fiber polysulfone membrane ultrafiltration to remove impurities, the inlet pressure is 0.2MPa, 200D hollow fiber polysulfone membrane nanofiltration is concentrated, the inlet pressure is 2.0MPa, and placed for crystallization.

[0023] Mix ethyl acetate-ethanol-water according to the volume ratio of 4:7:5, shake evenly by ultrasonic, stand and separate after layering, the lower phase is the solid phase, the upper phase is the mobile phase, the upper phase is used to dissolve the crystals, and the stationary phase Pump the chromatographic column fully, then adjust the speed of the main engine to 100rmp, and then pump the mobile phase at a flow rate of 2...

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PUM

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Abstract

The invention relates to a method for purifying ceylon leucas herb ketone by using high-performance countercurrent chromatography. The method comprises the following processing steps: a, crushing an anhydrous substance of ceylon leucas herb, carrying out ultrasonic extraction with ethanol, adding activated carbon to decolorize, and filtering; b, carrying out ultrafiltration and edulcoration on filtrate, carrying out nanofiltration concentration, placing and crystallizing; and c, separating a crystal substance by using high-performance countercurrent chromatography, and collecting a target composition according to a high performance liquid chromatography evaporative light scattering detector (HPLC-ELSD) test image. The method disclosed by the invention is simple in process, less in pollution, high in product purity, and applicable to industrial production.

Description

technical field [0001] The invention belongs to the field of separation of natural products, and relates to a method for purifying cellulone by using high-efficiency countercurrent chromatography. Background technique [0002] Honeycomb, also known as Dadujin, is derived from the whole herb of Lamiaceae Hydrangea and Parsnip. Honeycomb grass smells slightly bitter, tastes pungent, and has mild medicinal properties. [0003] Honeycomb is a commonly used Chinese herbal medicine. It is described in the "Common Chinese Herbal Medicine Handbook" of the Guangzhou Army: "Dispelling wind and relieving the exterior, relieving cough and reducing phlegm, treating colds, coughs, wind-fire toothache, gastrointestinal discomfort, and whooping cough"; "Wenshan Chinese Herbal Medicine" describes: " Relieving the exterior and relieving cough, improving eyesight and clearing the meridians; treating colds, headaches, stagnation, bronchial asthma, amenorrhea, indigestion, night blindness"; "Gu...

Claims

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Application Information

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IPC IPC(8): A61K36/53A61P1/00A61P31/04
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH