Method for supercritical fluid extraction of waxberry acid A

A technology of supercritical fluid and waxy myric acid, which is applied in the production of bulk chemicals and organic chemistry, can solve the problems that have not yet been reported on the production process of waxy myric acid A, and achieve easy large-scale production, large sample loading, and high yield. high rate effect

Inactive Publication Date: 2012-08-08
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, there is no report on the production process for preparing wax myricic acid A

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Take by weighing 1000g of Waxberry medicinal material and pulverize it into a coarse powder, put it into a supercritical extraction kettle, and use CO 2 As the solvent, set the temperature of the extraction column to 35°C and the pressure to 25MPa, the temperature of the separator to 30°C and the pressure to 5MPa, CO 2 The flow rate was 18L / h, the entrainer was added to ethanol solution with a volume fraction of 75%, the extraction time was 2h, and the extract was collected. Weigh the activated 200-300 mesh silica gel and put it into a stainless steel chromatography column (inner diameter 100mm, diameter-to-height ratio 1:12), dissolve the extract completely with methanol ultrasound, add it to the chromatography column, and use ethyl acetate- Elute with ethanol (15:1), collect the waxy myricate A fraction, concentrate under reduced pressure, cool and crystallize, filter to obtain coarse crystals, recrystallize with dichloromethane-methanol, filter out the crystals, and ...

Embodiment 2

[0018] Take by weighing 1000g of Waxberry medicinal material and pulverize it into a coarse powder, put it into a supercritical extraction kettle, and use CO 2 As the solvent, set the temperature of the extraction column to 42°C and the pressure to 37MPa, the temperature of the separator to 36°C and the pressure to 6MPa, CO 2 The flow rate is 20L / h, the entrainer is added to an ethanol solution with a volume fraction of 85%, the extraction time is 3h, and the extract is collected. Weigh the activated 200-300 mesh silica gel and put it into a stainless steel chromatography column (inner diameter 50mm, diameter-to-height ratio: 1:5), dissolve the extract completely with methanol ultrasound, add it to the chromatography column, and use ethyl acetate- Elute with ethanol (15:1), collect the waxy myricate A fraction, concentrate under reduced pressure, cool and crystallize, filter to obtain coarse crystals, recrystallize with dichloromethane-methanol, filter out the crystals, and dr...

Embodiment 3

[0020] Weigh 2000g of Waxberry medicinal material and pulverize it into a coarse powder, put it into a supercritical extraction kettle, and use CO 2 As the solvent, set the temperature of the extraction column to 50°C and the pressure to 45MPa, the temperature of the separator to 40°C and the pressure to 8MPa, CO 2 The flow rate was 22L / h, the entrainer was added to an ethanol solution with a volume fraction of 80%, the extraction time was 2.5h, and the extract was collected. Weigh the activated 200-300 mesh silica gel and put it into a stainless steel chromatography column (inner diameter 150mm, diameter-to-height ratio 1:18), dissolve the extract completely with methanol ultrasound, add it to the chromatography column, and use ethyl acetate- Elute with ethanol (15:1), collect the waxy myricate A fraction, concentrate under reduced pressure, cool and crystallize, filter to obtain coarse crystals, recrystallize with dichloromethane-methanol, filter out the crystals, and dry to...

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PUM

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Abstract

The invention discloses a method for supercritical fluid extraction of waxberry acid A, which comprises the steps of crushing raw materials, adopting supercritical fluid extraction, adding extract into a medium pressure silica gel column for chromatographic purification, performing ethyl acetate-ethanol elution, collecting the waxberry acid A flow, reducing pressure, concentrating and recrystalizing to obtain the waxberry acid A. The preparation method for the supercritical fluid extraction of the waxberry acid A is simple, suitable for large-scale production, low in energy consumption and small in pollution, and is environment-friendly type production process.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine chemistry and relates to a method for extracting waxy myric acid A with a supercritical fluid. Background technique [0002] Wax myriceric acid A (Myriceric acid A) molecular formula is C 39 h 52 o 7 , the molecular weight is 632.84. Colorless flaky crystals (methanol-water 8:2), mp.211-213°C. Wax Myrica rubra Myrica cerifera A triterpenoid compound was isolated from L. twigs. Pharmacological studies have shown that wax myricic acid A has endothelin receptor (ETA) antagonistic activity, and in rat aortic smooth muscle cells (A7r5), inhibits the combination of endothelin and A7r5, IC 50 0.04μg / mL; inhibit endothelin-induced Ca 2+ Mobile IC 50 0.0075μg / mL. [0003] In the prior art, there is no report on the production process for preparing waxy myricic acid A. Contents of the invention [0004] The purpose of the present invention is to provide a method for supercr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/00
CPCY02P20/54
Inventor 刘东锋郭琴
Owner NANJING ZELANG MEDICAL TECH
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