MPLC (medium-pressure liquid chromatography) separation and purification method for koumine

A technology for the preparation of liquid phase of keloids, which is applied in the field of industrial preparation of keloids, can solve the problems of long separation cycle, low recovery rate, and only dagram level, and achieve long separation cycle, short separation cycle, and easy operation. easy effect

Inactive Publication Date: 2018-05-04
FUJIAN MEDICAL UNIV
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  • Description
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Problems solved by technology

The disadvantages of column chromatography are long separation period, low recovery rate, large amount of solvent and difficult recovery, which is not conducive to environmental protection; the single preparation amount of high-speed countercurrent chromatography instrument is only in the order of several grams

Method used

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  • MPLC (medium-pressure liquid chromatography) separation and purification method for koumine

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Effect test

Embodiment 1

[0027] 1. Sample: Crude Gelkinsin, which is the total alkaloids of Gelkins extracted from Gelkins (Xu Jian, Liang Chongzhen. Comparison of extraction methods of Gelkins total alkaloids [J]. Pharmacy Bulletin, 1988, 23(6) :341-342.), the purity of glucuronine is 17%. The crude kelezin was dissolved in methanol, prepared to a concentration of 25 mg / mL, and passed through a 0.45 µm organic filter to obtain a sample solution.

[0028] 2. Instrument: Jiangsu Lisui Dr flash II medium pressure preparative liquid chromatograph.

[0029] 3. Elution solvent: methanol-water volume ratio (50︰50~80︰20) gradient elution solvent system.

[0030] 4. Separation and purification: first balance the chromatographic column in the medium-pressure preparative chromatograph packed in step 2 with methanol-water volume ratio (50:50), adjust the pump flow rate to 12 mL / min, and detect the wavelength at 256 nm . After pumping 10 mL of sample solution into the chromatographic column, gradient elution w...

Embodiment 2

[0032] 1. Sample: crude kinesin, which is the total alkaloids of kinesin extracted from kinesin (Zhang Lanlan. Extraction and separation of kinesin in total alkaloids of kinesin[J]. Journal of First Military Medical University, 2004, 24(9):1006-1008.), the purity of kelp is 22%. The crude kelezin was dissolved in methanol, prepared to a concentration of 25 mg / mL, and passed through a 0.45 µm organic filter to obtain a sample solution.

[0033] 2. Instrument: Jiangsu Lisui Dr flash II medium pressure preparative chromatograph.

[0034] 3. Elution solvent: methanol-water volume ratio (50︰50~80︰20) gradient elution solvent system.

[0035] 4. Separation and purification: first equilibrate the packed chromatographic column with methanol-water volume ratio (50:50), adjust the pump flow rate to 12 mL / min, and detect the wavelength at 256 nm. After pumping 10 mL of the sample solution into the chromatographic column, gradient elution with methanol-water (50︰50~80︰20) was carried ou...

Embodiment 3

[0037] 1. Sample: Crude Gelkinin, which is low-purity Gelkinin (26% pure) extracted from Gelkins (Zhao Qingchun, Guo Tao, Zhang Ping. Research on the separation and purification of total alkaloids of Gelkins by macroporous adsorption resin [J]. Chinese Pharmacy, 2006,17(13):969-971.). The crude kelezin was dissolved in methanol, prepared to a concentration of 25 mg / mL, and passed through a 0.45 µm organic filter to obtain a sample solution.

[0038] 2. Instrument: Jiangsu Lisui Dr flash II medium pressure preparative chromatograph.

[0039] 3. Elution solvent: methanol-water volume ratio (50︰50~80︰20) gradient elution.

[0040] 4. Separation and purification: first equilibrate the packed chromatographic column with methanol-water volume ratio (50:50), adjust the pump flow rate to 12 mL / min, and detect the wavelength at 256 nm. After pumping 10 mL of the sample solution into the chromatographic column, gradient elution with methanol-water (50︰50~80︰20) was carried out for 150...

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Abstract

The invention discloses an MPLC (medium-pressure liquid chromatography) separation and purification method for koumine. The method is characterized by comprising the following steps: 1) preparing a loading solution and an elution solvent system; 2) filling a chromatographic column with filler; 3) adding the loading solution, performing gradient elution, collecting eluates of corresponding absorption peaks according to appearance time, detecting the eluates with high-performance liquid chromatography, combining the eluates containing the koumine, and performing reduced-pressure evaporation andethanol recrystallization to obtain a koumine monomer. The loading solution is prepared through the following steps: total gelsemium alkaloids or low-purity koumine are or is dissolved in an organic solvent, and a sample solution is filtered by an organic filter membrane. The filler of the chromatographic column is normal-phase or reverse-phase silica gel filler. Compared with the traditional column chromatography and high-speed counter-current methods, the separation and purification method for the koumine has the advantages of being simple and convenient to operate and good in controllability. Medium-pressure preparative chromatographs with different specifications can be selected for separation, the preparation amount can reach hectogram scale, and industrial manufacture requirements can be met.

Description

technical field [0001] The invention relates to the field of industrial preparation of kelezin, in particular to a method for separating and purifying kelistin from alkaloids by using medium-pressure preparative liquid chromatography. Background technique [0002] hook kiss ( Gelsemium elegans Benth.) Nutriaceae vine is an evergreen woody vine. The whole plant is used as medicine, which has the effects of "reducing swelling and pain, dispelling wind and blood stasis, attacking poison and killing insects". The main active ingredients of Gelkins are indole alkaloids, which have pharmacological effects such as anti-inflammatory and analgesic, anti-tumor, anti-psoriasis, and promoting the growth of poultry and livestock. So far, there are 98 kinds of kelezin alkaloid monomers, among which kelezin is the monomer with the highest content and low toxicity. Kiskinin has high-efficiency, low-toxicity analgesic and anti-anxiety effects, and has a good medicinal prospect. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
Inventor 俞昌喜许盈石冬梅苏燕评游文兵
Owner FUJIAN MEDICAL UNIV
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