Preparation method for high-purity nitidine chloride as well as quality control method of high-purity nitidine chloride

A technique for chlorinated nephrine and a quality control method, which is applied in the field of high-purity chlorinated fenugreek preparation and its quality control, and can solve the problem that the chemical reference substance of high-purity chlorinated fenugreek cannot be satisfied, and there is no chlorinated fenugreek. The purity and quality control methods of needle alkali, the purity is not achieved, etc., to achieve the effect of reasonable design, quality assurance, and fast separation speed

Inactive Publication Date: 2013-05-08
广西新桂环保科技集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although people study and extract the method of chlorinated chlorinated amphadin at present, there are many methods, and various methods are different, but many methods for extracting chlorinated cinnamon have the disadvantages of low purity, low yield or high production cost, and the purity is average. It did not meet the requi...

Method used

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  • Preparation method for high-purity nitidine chloride as well as quality control method of high-purity nitidine chloride
  • Preparation method for high-purity nitidine chloride as well as quality control method of high-purity nitidine chloride
  • Preparation method for high-purity nitidine chloride as well as quality control method of high-purity nitidine chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Grind the roots of Acupunctus lanceolata into coarse powder, add 80% ethanol with pH=3 to reflux and extract three times, add 10 times the amount of acidic ethanol for the first time, heat and reflux for 2 hours; add acidic ethanol 5 times for the second and third times Double the amount, heat and reflux for 2 hours respectively; combine the acid-alcohol extracts, recover ethanol, continue to concentrate to a thick paste, grind repeatedly with chloroform, dissolve the obtained precipitate with methanol, add hydrochloric acid to pH 2, and precipitate light yellow-green needles after standing Recrystallized with methanol, it is a crude crystal of dihedral chloride. The hydrochloric acid weight content of the acidic ethanol is 10-30% hydrochloric acid, the ethanol weight content is 40-80%, and the pH=3-4.

[0046] (2) The crude product of chlorinated acantholine was then dissolved in methanol, ultrasonicated for 30 minutes, heated to 90°C, filtered while it was hot, le...

Embodiment 2

[0048] Example 2: (1) Grind the roots of Acupunctus acutilis into coarse powder, add 70% ethanol with pH=3 to reflux and extract three times, add 12 times the amount of acidic ethanol for the first time, heat and reflux for 3 hours; the second and third times Add 6 times the amount of acidic ethanol, heat and reflux for 3 hours respectively; combine the acid-alcohol extracts, recover the ethanol, continue to concentrate to a thick paste, grind repeatedly with chloroform, dissolve the obtained precipitate with methanol, add hydrochloric acid until the pH is 2, and precipitate after standing Pale yellow-green needle-like crystals, recrystallized with methanol, is coarse crystals of dihedral chloride. The hydrochloric acid weight content of the acidic ethanol is 10-30% hydrochloric acid, the ethanol weight content is 40-80%, and the pH=3-4.

[0049] (2) The crude product of chlorinated acantholine was dissolved in methanol, ultrasonicated for 40 minutes, heated to 95°C, filtered ...

Embodiment 3

[0051] Example 3: (1) Grind the root of Acupunctus acutilis into a coarse powder, add 50% ethanol with pH=4 to reflux and extract three times, add 15 times the amount of acidic ethanol for the first time, heat and reflux for 2 hours; the second and third times Add 5 times the amount of acidic ethanol, heat and reflux for 5 hours respectively; combine the acid-alcohol extracts, recover the ethanol, continue to concentrate to a thick paste, grind repeatedly with chloroform, dissolve the obtained precipitate with methanol, add hydrochloric acid until the pH is 3, and precipitate after standing Pale yellow-green needle-like crystals, recrystallized with methanol, is coarse crystals of dihedral chloride. The hydrochloric acid weight content of the acidic ethanol is 10-30% hydrochloric acid, the ethanol weight content is 40-80%, and the pH=3-4.

[0052] (2) The crude product of chlorinated acantholine was dissolved in methanol, ultrasonicated for 60 minutes, heated to 80°C, filtered...

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Abstract

The invention discloses a preparation method for high-purity nitidine chloride as well as a quality control method of high-purity nitidine chloride. The preparation method is characterized by comprising the following steps of: crushing radix zanthoxyli roots, heating up, refluxing and extracting by using acid alcohol; repeatedly grinding alcohol extract by chloroform; dissolving the obtained precipitates by using methanol, adjusting pH of the solution by using hydrochloric acid, and obtaining nitidine chloride coarse crystals by recrystallization; carrying out recrystallization by using methanol for further improving the purity; preparing by using reverse phase silica gel C-18 and separating by using high-performance liquid chromatography; detecting every part of collected eluant by utilizing an analysis type high performance liquid chromatograph; combining nitidine chloride components with the same retention time, and purity of 90%-98% and more than 98%; concentrating under reduced pressure to obtain nitidine chloride components with purity of 90%-98% and nitidine chloride components with purity bigger than 98%; and carrying out quality control by adopting a thin-layer chromatographic analysis method and a liquid-phase chromatographic analysis method. According to the preparation method disclosed by the invention, not only can the purity of the nitidine chloride be improved, but also the production cost can be reduced.

Description

technical field [0001] The invention relates to the field of natural medicines, in particular to a preparation and quality control method of high-purity cinnamon chloride. Background technique [0002] Zanthoxylum nitidum (Roxb.) DC., the dry root of Zanthoxylum nitidum (Roxb.) DC., belongs to the dry root of Rutaceae Zanthoxylum nitidum. One, it has good effects of promoting qi and relieving pain, promoting blood circulation and removing blood stasis, dispelling wind and dredging collaterals. It is the first choice of commonly used drugs by medical experts, and is widely used in traditional Chinese medicine prescriptions, Chinese patent medicines and fine chemical products. In recent years, the annual demand has been increasing. Products using LMZ herbs as raw materials include nationally famous brands "LMZ TCM Toothpaste", "Sanjiu Weitai", "Jinji Capsule", "Compound LMZ Lozenges", "LMZ Zhen Pain Tablets", "Gushui", "Zhonghua Dieda Pills", "Huoluo Zhitong Pills" and many o...

Claims

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Application Information

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IPC IPC(8): C07D491/056G01N30/90G01N30/02
Inventor 刘布鸣黄艳赖茂祥莫建光柴玲林霄陈明生
Owner 广西新桂环保科技集团有限公司
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