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A method for photocatalytic enrichment of low-content α-asarone and its application

A photocatalytic reactor, asarum technology, which is used in ether separation/purification, ether preparation, organic chemistry, etc., can solve the problems of difficult separation and preparation, achieve high output per unit time, improve extraction rate, and improve separation efficiency Effect

Active Publication Date: 2022-04-05
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problem in the prior art that the content of α-asarone in the medicinal material of Shichangpu is low, less than 1 / 30 of β-asarone, and it is difficult to separate and prepare a large amount of it, the purpose of this disclosure is to develop a preparation cost It is lower than the existing technology, easy to operate, high in efficiency, can efficiently photocatalyze enrichment from Acorus calamus in large batches, and separate and prepare asarone monomer components with a purity greater than 98%

Method used

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  • A method for photocatalytic enrichment of low-content α-asarone and its application
  • A method for photocatalytic enrichment of low-content α-asarone and its application
  • A method for photocatalytic enrichment of low-content α-asarone and its application

Examples

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Embodiment 1

[0054] This example provides a method for extracting α-asarone from Acorus calamus.

[0055] 1. Sample Extraction

[0056] Dry the rhizomes of Acorus calamus and crush them to different particle sizes. Precisely weigh 2g of medicinal material powder and place it in the extraction kettle. Add a filter membrane to the bottom of the extraction kettle in advance, place the extraction kettle on the fixing device of the extraction kettle, and close the door of the extraction kettle. Using n-hexane as the extraction solvent, set the parameters of the accelerated solvent extraction method, including extraction solvent (n-hexane, ethyl acetate, methanol, water), sample particle size (10-20 mesh, 20-30 mesh, 30-60 mesh, 60–80 mesh, >80 mesh), extraction temperature (80°C, 100°C, 120°C, 140°C), cycle times (1 time, 2 times, 3 times), static extraction time (6min, 8min, 10min, 12min ), etc., start the accelerated solvent extraction apparatus, stop automatically after the extraction is co...

Embodiment 2

[0082] This embodiment carries out purity analysis and structure identification to the product obtained in embodiment 1

[0083] The purity analysis was carried out by high performance liquid chromatography, and the high performance liquid chromatography was carried out by C 18 Chromatographic column (250mm×4.6mm, 5μm), flow rate 1.0mL / min; column temperature 25°C; detection wavelength: 254nm, injection volume 10μL. Gradient analysis mobile phase: methanol / water=60:40 (v / v).

[0084] Purity analysis and structural characterization were carried out by high performance liquid chromatography, mass spectrometry and nuclear magnetic resonance techniques. The scanning range is m / z 100-1000, and the deuterium reagent is chloroform.

[0085]α-Asarone: ESI-MS, m / z209.1178[M+H] + .1H-NMR (400MHz, CDCl 3 )δ:1.83 (3H,dd,J=1.5,7.5Hz,H-30),3.77,3.82,3.86(each,3H,s,OCH 3 ),5.74(1H,dq,J=7.2,11.4,H-20),6.50(1H,dq,br d,H-10),6.53(1H,s,H-3),6.84(1H,s, H-6). 13 C-NMR (100MHz, CDCl 3 )δ: 1...

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Abstract

The disclosure relates to the technical field of compound extraction, and specifically provides a low-content α-asarone photocatalytic enrichment and application thereof. The method comprises the following steps: adding the total extract of Shichangpu to a selected solvent, placing it in a photocatalytic reactor for reaction, after the reaction is completed, evaporating the solvent to dryness under reduced pressure to obtain a photoconverted product of the total sample of Shichangpu, the total sample of Shichangpu In the photoconverter, part of β-asarone is converted into α-asarone. It solves the problems in the prior art that the content of α-asarone in Acorus calamus is relatively low, less than 1 / 30 of that of β-asarone, and it is difficult to separate and prepare a large amount.

Description

technical field [0001] The disclosure relates to the technical field of compound extraction, and specifically provides a method for photocatalytic enrichment of low-content α-asarone and its application. Background technique [0002] The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art. [0003] Acorus tatarinowii Schott (Latin name: Acorus tatarinowii Schott) is the dried rhizome of Acorus tatarinowii Schott, a perennial herb of the family Araceae. Modern pharmacological studies have shown that the active ingredient volatile oil of Shichangpu has regulatory effects on the central nervous system, cardiovascular, respiratory and digestive systems, and its main active ingredients are β- and α-asarone. The quality control of Acorus calamus medicinal materials, the optimization of the production process and quality control of finished medicines play an important role. At the same time, α-asar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/32C07C41/36C07C43/215
Inventor 孙蓉王岱杰黄娜娜崔莉赵恒强张新雨刘闰平李晓骄阳
Owner SHANDONG UNIV