Method for separating effective ingredient lagehead atractylodes lactone III from lagehead atractylodes naphtha

A technique for volatile oil of Atractylodes Rhizoma and Atractylodes Rhizoma Lactone is applied in the field of traditional Chinese medicine, which can solve the problems of difficulty in industrialization, time-consuming and labor-intensive, etc., and achieve the effect of simple operation.

Inactive Publication Date: 2006-02-15
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The commonly used method for separating Atractylodes lactone III in the literature is column chromatography, which is time-consuming and laborious, and difficult to industrialize

Method used

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  • Method for separating effective ingredient lagehead atractylodes lactone III from lagehead atractylodes naphtha
  • Method for separating effective ingredient lagehead atractylodes lactone III from lagehead atractylodes naphtha

Examples

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Effect test

Embodiment 1

[0023] Dry Atractylodes Rhizome (Xinchang, Zhejiang) naturally, crush it, take Atractylodes Rhizoma Atractylodes Rhizoma Rhizome, and soak it with 6 times the volume of ethyl acetate for 3 times (1 hour each time, in a constant temperature water bath at 70°C, with a stirring speed of 500r / min), and recover the solvent to obtain a yellowish brown color. Volatile oil. The volatile oil was dissolved in methanol and placed at 0°C for 24 hours to remove insoluble matter, and the filtrate was distilled under reduced pressure to obtain refined volatile oil. The volatile oil was dissolved with 2 times the volume of ethyl acetate, and then petroleum ether (60-90° C.) was gradually added until the final volume concentration reached 80%, and the precipitate was removed. Concentrate the filtrate by distillation under reduced pressure and degrease with 8 times the volume of petroleum ether (60-90°C) for 4 times (each time for 1h, 60°C constant temperature water bath, stirring speed 300r / mi...

Embodiment 2

[0025] Dry Atractylodes Rhizome (Xinchang, Zhejiang) in an oven at 60°C, crush it, take Atractylodes Rhizoma Atractylodes Rhizoma Rhizome, and soak it with 8 times the volume of dichloromethane at room temperature for 3 times (1 hour each time, stirring speed 400r / min), and recover the solvent to obtain a yellowish brown color. Volatile oil. The volatile oil was dissolved in absolute ethanol and placed at -4°C for 24 hours to remove insoluble matter, and the filtrate was distilled under atmospheric pressure to obtain refined volatile oil. The volatile oil was dissolved with 2 times the volume of dichloromethane, and then n-hexane was gradually added until the final volume concentration reached 90%, and the precipitate was removed. Concentrate the filtrate by distillation under reduced pressure and use 4 times the volume of n-hexane to degrease at room temperature for 3 times (1h each time, 500r / min), and recrystallize (n-hexane-dichloromethane volume ratio 9:1) to obtain Atra...

Embodiment 3

[0027] Dry Atractylodes Rhizome (Xinchang, Zhejiang) naturally, crush it, take Atractylodes Rhizoma Atractylodes Rhizoma Atractylodes Rhizome and extract it twice in a Soxhlet extraction device with 8 times the volume of chloroform (3 hours each time), and recover the solvent to obtain a yellow-brown volatile oil. The volatile oil was dissolved in propanol and placed at -2°C for 24 hours to remove insoluble matter, and the filtrate was concentrated by vacuum distillation to obtain refined volatile oil. The volatile oil was dissolved with 2 times the volume of chloroform, and then cyclohexane was gradually added until the final volume concentration reached 85%, and the precipitate was removed. Concentrate the filtrate by atmospheric distillation and degrease 3 times with 6 times the volume of cyclohexane (each time for 1h, 60°C constant temperature water bath, stirring speed 300r / min), carry out recrystallization (cyclohexane-chloroform volume ratio 10:1 ), the colorless needle...

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Abstract

The invention discloses a process for separating effective component of butenolide III from lagehead atractylodes volatile oil, which comprises leaching the disintegrated lagehead atractylodes with medium polar solvent, reclaiming the solvent to obtain chartreuse green volatile oil, dissolving the volatile oil with low carbon chain and storing at -4 to 0 deg C, removing insoluble substances, concentrating the filtrate to obtain refined volatile oil, dissolving the volatile oil with medium polar solvent, then gradually charging low polar solvent, removing precipitation, concentrating the filter liquor and degreasing with low polar solvent, finally carrying out recrystallization.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicines, and in particular relates to a method for separating the active ingredient atractylodes lactone III from the volatile oil of atractylodes rhizome. Background technique [0002] Atractylodes macrocephala is a traditional Chinese medicinal material, which is the dried rhizome of Atractylodes macrocephala Koidz. Atractylodes macrocephala, also known as Yushu, Dongzhu, Zheshu, etc., is a perennial herb. Its nature is warm, sweet and bitter. It has the functions of invigorating the spleen and replenishing qi, drying dampness and diuresis, antiperspirant, and preventing miscarriage. It is mainly used for spleen deficiency, indigestion, abdominal distension and diarrhea, fatigue and weakness, phlegm retention, dizziness, edema, spontaneous sweating, restless fetal movement, and is an essential medicine for invigorating the spleen in traditional Chinese medicine. Modern pharmacological res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/92
Inventor 何潮洪赵春霞
Owner ZHEJIANG UNIV
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