Method for extracting hydroxyl sanshool from zanthoxylum oil

A technology of hydroxyl sanshool and prickly ash oil, which is applied in the field of extracting bioactive components, and achieves the effects of convenient operation, simple pretreatment and high purity

Active Publication Date: 2012-09-26
汉源县昊业科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But unfortunately, there is no existing bibliographical report to separate and purify the method of these two sanshools from Zanthoxylum bungeanum oil

Method used

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  • Method for extracting hydroxyl sanshool from zanthoxylum oil
  • Method for extracting hydroxyl sanshool from zanthoxylum oil
  • Method for extracting hydroxyl sanshool from zanthoxylum oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 20 ml of Zanthoxylum bungeanum oil into methanol at a volume ratio of 1:20, mechanically shake at room temperature for 20 minutes, then ultrasonically shake at an ultrasonic frequency of 35Hz for 5 minutes, and then centrifuge the extract at a speed of 2500r / min for 10 minutes ; Take supernatant, pass Al 2 o 3 After the polyphenols were removed by the chromatographic column, it was frozen at -20°C in the dark for 12 hours; the extract was subjected to rotary evaporation at ≤40°C to obtain 0.95 g of the concentrate.

[0023] First dissolve the concentrate with 3 ml of 70% (v / v) methanol, and load the sample according to the mass ratio of the sample to the silica gel column at 1:40, and then use 70% (v / v) methanol as the eluent at an elution flow rate of Perform isocratic elution at 0.5ml / min, and collect the eluate in 120 ml aliquots, and combine with thin-layer chromatography. Under the ultraviolet light of 254 nm, the second group with obvious purple spots appears...

Embodiment 2

[0028] Add 30 ml of Zanthoxylum bungeanum oil into methanol at a volume ratio of 1:25, first shake mechanically at room temperature for 25 minutes, then ultrasonically shake at an ultrasonic frequency of 45 Hz for 8 minutes, and then centrifuge the extract at a speed of 2800 r / min for 12 minutes; Take supernatant, pass Al 2 o 3 After the polyphenols were removed by the chromatographic column, it was frozen at -20°C in the dark for 15 hours; the extract was subjected to rotary evaporation at ≤40°C to obtain 1.275 g of the concentrate.

[0029] First dissolve the concentrate with 3.5 ml of 75% (v / v) methanol, and load the sample according to the mass ratio of the sample to the silica gel column at 1:45, and then use 75% (v / v) methanol as the eluent at an elution flow rate of The isocratic elution was performed at 1ml / min, and the eluate was collected in 100ml aliquots according to the collection volume of each part, and combined with thin layer chromatography, the second compon...

Embodiment 3

[0034]Add 40 ml of Zanthoxylum bungeanum oil into methanol at a volume ratio of 1:30, mechanically shake at room temperature for 30 minutes, then ultrasonically shake at an ultrasonic frequency of 55 Hz for 10 minutes, and then centrifuge the extract at a speed of 3000 r / min for 15 minutes; Supernatant, over Al 2 o 3 After the polyphenols were removed by the chromatographic column, it was frozen below -20°C in the dark for 18 hours; the extract was subjected to rotary evaporation at ≤40°C to obtain 1.901 g of a concentrate.

[0035] First dissolve the concentrate with 4 ml of 80% (v / v) methanol, and load the sample according to the mass ratio of the sample to the silica gel column at 1:50, and then use 80% (v / v) methanol as the eluent to elute at a flow rate of 1.5 ml / min for isocratic elution, and the eluate was collected in 80ml aliquots according to the collection volume of each part, and combined with thin layer chromatography, the second component with obvious purple spo...

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Abstract

The invention discloses a method for extracting hydroxyl sanshool from zanthoxylum oil. The process comprises the following steps of: 1) extracting zanthoxylum oil by using methyl alcohol at room temperature, performing centrifugal separation, performing chromatography to remove polyphenol, freezing, and performing rotary evaporation to obtain concentrate; 2, dissolving concentrate in methyl alcohol, performing gradient elution by using a silicagel column, collecting equally divided parts of eluent, and concentrating and drying an aimed compound which is initially determined by thin-layer chromatography; and 3) subdividing and purifying the obtained concentrate by using preparative liquid chromatography, collecting the eluent of the two maximum absorption peaks respectively, and performing rotary evaporation to obtain hydroxyl sanshool I and II. The method fills the blank of the prior art, provides standard substance for quantifying the numb tastes of zanthoxylum for the field, and is convenient to operate; and the pretreatment is easy to realize; and substance obtained through separation and purification is high in purity.

Description

technical field [0001] The invention belongs to the technical field of extracting bioactive components from plants of the genus Zanthoxylum, in particular to a method for extracting hydroxy sanshool from Zanthoxylum oil. Background technique [0002] Zanthoxylum bungeanum oil refers to soaking Zanthoxylum bungeanum directly with edible oil or using organic solvent extraction, supercritical CO 2 The seasoning oil with hemp flavor is made by mixing the pepper oleoresin prepared by extraction and other methods with edible oil in an appropriate amount. Since the processing of Zanthoxylum bungeanum oil greatly reduces the loss of active ingredients and microbial contamination caused by Zanthoxylum bungeanum during storage and sales, and solves the inconvenience caused by Zanthoxylum bungeanum and Zanthoxylum powder to cooking and eating, it is more and more popular among consumers. However, the current pepper oil market is not regulated, and most of the product labels only indic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/20
Inventor 赵志峰祝瑞雪钟凯高鸿温建镇
Owner 汉源县昊业科技有限公司
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