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Method for quickly preparing high-content zanthoxylum unsaturated amide components

An unsaturated and amide technology, which is applied in the field of rapid preparation of high-content unsaturated amide components, can solve the problems of easy oxidative deterioration, hindered application, no commodity supply, etc., and achieves simple and reliable method, small preparation amount, fast and effective. Extraction and separation effects

Inactive Publication Date: 2014-09-10
NANJING INST FOR THE COMPREHENSIVE UTILIZATION OF WILD PLANTS CHINA COOP
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  • Claims
  • Application Information

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Problems solved by technology

However, due to the complex components in Zanthoxylum bungeanum, the separation and purification of unsaturated amides is mainly prepared by column chromatography. At the same time, because the structure of long-chain unsaturated fatty acids in unsaturated amides is very unstable, it is easily oxidized in the air This series of factors lead to technical bottlenecks in the large-scale preparation of high-content unsaturated amides. There is no commercial supply of reference substances for the quantitative analysis of Zanthoxylum bungeanum flavor components, and there is a lack of effective quality evaluation methods for Zanthoxylum bungeanum and its products. Means, while hindering its wider and deeper application in the fields of medicine and food

Method used

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  • Method for quickly preparing high-content zanthoxylum unsaturated amide components
  • Method for quickly preparing high-content zanthoxylum unsaturated amide components

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Embodiment 1: take by weighing 50g content and be the supercritical CO of 50% 2 Add 300mL of petroleum ether to the red pepper oleoresin produced by the extraction method, stir and dissolve at 5°C for 3 hours, repeat 3 times in total, obtain 31.2g of solid residue after vacuum filtration at 5°C; add 250mL of hexane to the solid residue, Heated and refluxed extraction, extracted 3 times, filtered while hot; the filtrate was frozen at -20°C for 24 hours, vacuum filtered at 5°C to obtain white crystals, washed with a small amount of hexane, vacuum filtered at -5°C, and the obtained crystals were released Put it into a desiccator and blow and dry it with high-purity nitrogen at -5°C for 20 minutes and seal it for storage to obtain high-content unsaturated amide crystals of Zanthoxylum bungeanum. According to high-performance liquid phase analysis, the content is 96.9%.

Embodiment 2

[0014] Example 2: Weigh 100g of 30% ethanol-extracted red prickly ash oleoresin, add 800mL No. 6 solvent oil, stir and dissolve at 15°C for 2h, repeat 3 times, and obtain 52.8g of solid residue after vacuum filtration at 4°C; Add 600mL cyclohexane to the solid residue, heat and reflux at 80°C for extraction, extract 3 times, and quickly filter while hot; freeze the filtrate at -15°C for 24 hours, vacuum filter at 0°C to obtain white crystals, and wash with cyclohexane , vacuum filtration at 0°C, put the obtained crystals into a desiccator and purge and dry them with high-purity nitrogen at 0°C for 25 minutes and seal them for storage to obtain high-purity unsaturated amide crystals of Zanthoxylum bungeanum, which were analyzed by high-performance liquid phase, and the content was 95.2 %.

Embodiment 3

[0015] Embodiment 3: take by weighing 150g content and be the supercritical CO of about 40% 2 Add 1000mL of n-hexane to the green pepper oleoresin produced by the extraction method, stir and dissolve at 25°C for 3 hours, repeat 3 times in total, obtain 87.4g of solid residue after vacuum filtration at 30°C; add 1000mL of isooctane to the solid residue, heat at 90°C Reflux extraction, extract 3 times, and quickly filter while hot; freeze the filtrate at -10°C for 24 hours, and vacuum filter at 5°C to obtain white crystals, then wash with isooctane, vacuum filter at 5°C, and place the obtained crystals in a dry place. The device was purged and dried with high-purity nitrogen at 5°C for 30 minutes and sealed for storage to obtain high-purity unsaturated amide crystals of Zanthoxylum bungeanum, which was analyzed by high performance liquid phase, and the content was 95.7%.

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Abstract

The invention discloses a method for quickly preparing high-content zanthoxylum unsaturated amide components. The method comprises the following steps: (1) adding a low-polar solvent into zanthoxylum oleoresin serving as a raw materials, stirring and filtering to obtain solid residues; (2) adding one or more of hexane, cyclohexane and isooctane into the solid residues, heating, performing reflux extraction, and filtering; (3) freezing and crystallizing the filtrate at minus 10- minus 20 DEG C; (4) washing and filtering the crystal, purging and drying in high-purity nitrogen at negative 5-5 DEG C to obtain high-content zanthoxylum unsaturated amide components. According to the method, application of column chromatography in the prior art can be avoided, the high-content unsaturated amide components can be quickly and effectively prepared, and the method is simple and reliable at low cost. Mass spectrum identifies that the prepared crystal sanshool and isomerides, the content detected by high-performance liquid chromatography is over 95 percent, and the crystal can meet basic requirements for reference substance application in the aspects of content detection, quality evaluation and the like.

Description

technical field [0001] The invention relates to a rapid preparation method of high-content unsaturated amide components in Zanthoxylum bungeanum. Background technique [0002] Zanthoxylum bungeanum refers to red pepper ( Zanthoxylum Bungeanum Maxim) and green peppercorns ( Zanthoxylum armatum v. novemfolius ) dry ripe fruit peel, belonging to Rutaceae ( Rutaceae ) Zanthoxylum ( Zanthoxylum ), which is a unique spice resource in my country. The characteristic aroma and numbing taste of Zanthoxylum bungeanum make it widely used in cooking seasoning of various cuisines, especially Sichuan cuisine [2] , giving dishes a unique flavor. [0003] The main chemical components in Zanthoxylum bungeanum are volatile oil, amides, alkaloids, etc. Among them, the two flavor components of volatile oil and amides reflect the aroma and numbness characteristics of Zanthoxylum bungeanum, and they are also the two most important characteristic indicators in the quality evaluation of Z...

Claims

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Application Information

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IPC IPC(8): C07C233/20C07C231/24
CPCY02P20/54
Inventor 赵伯涛张卫明朱羽尧张国琳钱骅黄晓德陈斌
Owner NANJING INST FOR THE COMPREHENSIVE UTILIZATION OF WILD PLANTS CHINA COOP
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