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Method for preparing nitidine chloride from total alkali extract of zanthoxylum nitidum stems and branches

A technology of chlorinating limpet base and limpet, which is applied in organic chemistry and other fields, can solve the problems of large production consumption, and achieve the effect of fast separation speed and simple operation

Inactive Publication Date: 2018-08-31
GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, with the continuous deepening of research on the chemical components and pharmacological activities of LMZ, its uses have also been continuously expanded. However, the demand for LMZ medicinal materials is also increasing, and the traditional medicinal parts are basically unable to meet the needs due to the large amount of clinical and production. Therefore, if the stems and branches of LMZ can be fully utilized, the resources of LMZ can be fully and rationally utilized, and the medicinal value and economic benefits of LMZ can be greatly improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 0.5 kg of the stems and branches of limping needles, crush them into coarse powder, add 4.0 kg of 95% ethanol to reflux and extract twice, each time for 2 hours, combine the filtrates, recover the ethanol, concentrate to a thick paste, and obtain the total alkali extraction of the stems and branches of limping needles Compound 14.2g.

[0021] Take 14.2g of the total alkali extract of the above-mentioned stems and branches of Liangmianzhen, add 28.4g of methanol to dissolve, add 28.4g of column chromatography silica gel to mix the sample, mix well, evaporate to dryness, grind to powder, put it in the chromatography column, and mix it with acetic acid Ethyl-methanol is eluted, and the volume ratio of ethyl acetate and methanol is 8:2; According to total alkali extract quality: eluent volume=1g:20ml ratio collects eluent, to each part of eluent collected TLC was used to identify and track observations, select the eluents containing chlorinated amphetine, combine them,...

Embodiment 2

[0023] Take 1.0kg of the stems and branches of the double-sided needles, crush them into coarse powder, add 10.0kg of 95% ethanol to reflux extraction for 3 times, each time for 1 hour, combine the filtrates, recover the ethanol, concentrate to a thick paste, and obtain the total alkali extraction of the stems and branches of the double-sided needles Compound 25.3g.

[0024] Take 25.3g of the total alkali extract of the above-mentioned stems and branches of Liangmianzhen, add 75.9g of methanol to dissolve, add 75.9g of column chromatography silica gel to mix the sample, mix well, evaporate to dryness, grind to powder, put it in the chromatography column, and mix it with acetic acid Ethyl-methanol is eluted, and the volume ratio of ethyl acetate and methanol is 9:1, and according to total alkali extract quality: eluent volume=1g:20ml ratio collects eluent, to each part of eluent collected Adopt thin-layer identification and follow-up observation, select the eluent containing am...

Embodiment 3

[0026] Take 2.0kg of stems and branches of limping needles, crush them into coarse powder, add 24.0kg of 95% ethanol to reflux and extract once for 3 hours each time, combine the filtrates, recover ethanol, concentrate to a thick paste, and obtain the total alkali extraction of limping needles stems and branches Compound 51.4g.

[0027] Take 51.4g of the total alkali extract of the above-mentioned stems and branches of Liangmianzhen, add 304.2g of methanol to dissolve, add 304.2g of column chromatography silica gel to mix the sample, mix well, evaporate to dryness, grind to powder, put it in the chromatography column, and mix it with acetic acid Ethyl-methanol is eluted, and the volume ratio of ethyl acetate and methanol is 7:3, and according to total alkali extract quality: eluent volume=1g:20ml ratio collects eluent, to each part of eluent collected TLC was used to identify and track observations, select the eluents containing amphetine chloride, combine them, concentrate to...

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Abstract

The invention discloses a method for preparing nitidine chloride from a total alkali extract of zanthoxylum nitidum stems and branches. The method comprises the steps: adding an alcohol-water solventwith the amount 6-12 times the mass parts of the zanthoxylum nitidum stems and branches into the zanthoxylum nitidum stems and branches, carrying out reflux extraction for 1-3 times for 1-3 h each time, merging filtrates, recovering alcohol and concentrating to a thick paste, and thus obtaining the total alkali extract of the zanthoxylum nitidum stems and branches; adding column-layer chromatographic silica gel with the amount of 2-10 times that of the thick paste to the obtained thick paste, placing in a chromatography column, carrying out solid-liquid extraction separation with ethyl acetateand methanol, merging fractions with same results by thin layer chromatography, and carrying out repeated concentration, precipitation and suction filtration, to obtain a crude compound; recrystallizing with a methanol solvent to obtain a high-purity monomer compound, carrying out primary identification of the components of the monomer compound by thin layer chromatography and a melting point determination method, and identifying the monomer compound obtained from separation to be nitidine chloride according to the physical properties of the compound and thin layer identifying. The method forextracting nitidine chloride from zanthoxylum nitidum is simple and feasible, high in yield, simple to operate and high in separation efficiency.

Description

technical field [0001] The present invention belongs to, in particular, a method for preparing chlorinated alkaloids from the total alkaloid extract of limpet stems and branches. Background technique [0002] Zanthoxylum nitidum (Roxb.) DC. Also known as double-faced needle, double-backed needle, ground golden cow, manjiao, etc., is a vine of the genus Zanthoxylum in Rutaceae, distributed in Zhejiang, Fujian, Taiwan, Hunan, Guangdong, Hainan, In Guangxi, Sichuan, Yunnan and other places, it grows in low hills, bushes, roadsides and other sunny places. The traditional medicinal part of LMZ is the root, which is a commonly used traditional Chinese medicine in clinical practice. Its nature and flavor are pungent, bitter, slightly warm, slightly poisonous, and have the effects of expelling wind and dredging collaterals, eliminating dampness and relieving pain, reducing swelling and detoxification. In traditional Chinese medicine, it can treat rheumatic paralysis, bruises, swel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/056
CPCC07D491/056
Inventor 陆国寿蒋珍藕黄建猷赖茂祥黄周锋胡筱希
Owner GUANGXI INST OF CHINESE MEDICINE & PHARMA SCI
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