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Method for separating and purifying patchouli alcohol

A patchouli alcohol, separation and purification technology, applied in the field of separation and purification of natural active ingredients, to achieve the effect of simple and mature process, low cost and high yield

Active Publication Date: 2010-04-07
DONGGUAN MATHEMATICAL ENG ACAD OF CHINESE MEDICINE GUANGZHOU UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

How to purify patchouli alcohol from patchouli oil as a raw material for medicine has not yet been reported

Method used

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  • Method for separating and purifying patchouli alcohol
  • Method for separating and purifying patchouli alcohol
  • Method for separating and purifying patchouli alcohol

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0024] Experimental Example: Separation and Purification of Patchouli Alcohol in Patchouli Oil by Batch Rectification

[0025] 1. Experimental equipment

[0026] Distillation experimental equipment: using rectification tower inner diameter φ25mm, tower height 1.5m, φ3×3mm stainless steel e-shaped mesh ring packing; AL intelligent temperature control instrument; swing tower head, automatic control of reflux; 2XZ-0.5 vacuum pump; U type differential pressure gauge.

[0027] 2. Experimental method

[0028] The vacuum distillation experiment was carried out under the pressure of 745mmHg. Add patchouli oil 350g, turn on the cooling water switch, after ensuring that the cooling water is normal, turn on the electric heating mantle switch and start heating. The heating current is adjusted to 0.6A. After about 30 minutes, the temperature of the kettle rose to 134.8°C, and the patchouli oil began to boil. After 10 minutes, the temperature of the tower kettle reached 135.1°C, and re...

experiment example 2

[0041] Experimental Example 2 Separation and Purification of Patchouli Alcohol in Patchouli Oil by Vacuum Distillation

[0042] 1. Materials and equipment

[0043] 500mL distillation flask, 100mm thorn-shaped fractionation column, 400mm condenser tube, 500mL temperature-controlled electric heating mantle, connection tube, thermometer 100-300°C, 250mL buffer bottle, 2XZ-1 vacuum pump.

[0044] 2. Methods and Results

[0045] Set up the vacuum distillation device, get patchouli oil 250g, add in the distillation flask, heat, open vacuum 400Pa. When the gas phase temperature reaches 64°C, start discharging, adjust and control the temperature, maintain a uniform temperature gradient in the fractionation column, and control the speed of the distillate at about 2 to 3 seconds / drop, and obtain the component collectors The samples in the sample and the still liquid in the distillation flask were analyzed by gas chromatography, and the extraction rate and mass fraction of patchouli al...

experiment example 3

[0050] Experimental Example Trimolecular Distillation Separation and Purification of Patchouli Alcohol in Patchouli Oil

[0051] 1. Materials and equipment

[0052] Pope WFS wiped film molecular still

[0053] 2. Methods and results

[0054] Put 500g of patchouli oil into the molecular distillation device from the feeder, fill the cold trap with liquid nitrogen to protect the vacuum system, turn on the condensed water at 25°C, and when the required vacuum degree of 0.2Pa is reached, turn on the heat transfer oil system for precise control When the temperature of the evaporating surface is close to the set value, turn on the motor, adjust the scraping film rotor to an appropriate speed, and scrape the material evenly around the cylinder wall. Molecular distillation was carried out at an evaporation temperature of 75°C, a feed rate of 80mL / h, and a film scraping rate of 190r / min, and the sample in the heavy component collector was obtained for gas chromatographic analysis to c...

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Abstract

The invention provides a method for separating and purifying patchouli alcohol, which is used for industrially separating and purifying the effective component of patchouli alcohol in patchouli oil and can meet the requirements of the pharmaceutical industry. The method comprises the following steps: firstly, separating and extracting the patchouli alcohol from the patchouli oil by a rectification method and a distillation method to obtain a distillate or residue liquid containing over 40 mass percent of patchouli alcohol; standing a distillate or residue liquid containing over 70 mass percent of patchouli alcohol at room temperature or below, crystalizing and precipitating the distillate or the residue liquid to obtain patchouli alcohol crystals; filtering the patchouli alcohol crystals to obtain high purity patchouli alcohol crystals and filtrate after the crystallization; and adding a small amount of patchouli alcohol crystals into the filtrate, standing at room temperature or below, repeating the crystallization and filtration until crystals are not precipitated any more, and filtering to obtain high purity patchouli alcohol crystals. The method has simple and mature process, and is easy to realize the industrial production; the patchouli alcohol crystals obtained by separation have high purity; and the patchouli alcohol has high yield and low cost.

Description

technical field [0001] The invention relates to the technical field of separation and purification of natural active ingredients, in particular to a method for separating and purifying a single active ingredient patchouli alcohol (pothouli alcohol) from natural patchouli oil. Background technique [0002] Patchouli oil, also known as Baiqiu plum oil, is the volatile oil extracted from the Lamiaceae Patchouli plant Pogostemon cablin (Blanco) Benth. The 2005 edition of "Chinese Pharmacopoeia" records: Patchouli oil has the effects of aromatizing dampness, appetizing and relieving nausea, and relieving summer heat. Summer heat, abdominal pain, vomiting and diarrhea, nasal sinusitis headache embolism. Patchouli oil mainly contains patchouli alcohol and patchouli ketone (the total amount of the two accounts for more than 40%). The quality control of patchouli and patchouli oil in legal standards all use patchouli alcohol as the content determination index. Patchouli alcohol be...

Claims

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Application Information

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IPC IPC(8): C07C35/37C07C29/80C07C29/78
Inventor 赖小平苏子仁黎玉翠
Owner DONGGUAN MATHEMATICAL ENG ACAD OF CHINESE MEDICINE GUANGZHOU UNIV OF CHINESE MEDICINE
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