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A kind of Tingcetamine D, Tingcetamine E and its preparation method and application
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A kind of Tingli new amine, Tingli new amine technology, applied in Tingli new amine D, Tingli new amine E and the field of preparation thereof, to achieve the effects of scientific and reasonable preparation method, abundant raw materials, significant economic and social benefits
Active Publication Date: 2019-05-10
HENAN UNIV OF CHINESE MEDICINE
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[0004] In view of the above situation, in order to overcome the defects of the prior art, the object of the present invention is to provide a kind of Tinglisine D, Tinglisine E and their preparation method and application, which can effectively solve the problem of extracting Tinglisine from Tinglizi chinensis. Neoamine D, Tinglixinamine E and problems in preparing drugs for treating cardiomyocyte H9c2 injury
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[0032] The specific implementation of the present invention will be described in detail below in combination with specific situations.
[0033] In the specific implementation of the present invention, a kind of Tinglisine D, Tinglisine E and their preparation method and application, wherein the Tinglisine D molecular formula is C 20 h 22 N 2 o 5 , the molecular formula of Tinglisamine E is C 18 h 20 N 2 o 4 , the molecular formula is:
[0034]
[0035] The preparation method of this Tingcetamine D, Tingcetamine E is:
[0036]Take 10kg of Tinglizi, stir-fry at 240°C for 5.5 minutes, take the fried Tinglizi, add 10 times the weight of Tinglizi to decoct and extract three times, each time After 1.5h, the extract was concentrated under reduced pressure to an extract (5L) equivalent to 2g / mL of the crude drug. Then add 25L of ethanol with a volume concentration of 80% for alcohol precipitation, repeat the operation 4 times, concentrate the obtained supernatant until it ...
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Abstract
The invention relates to a semen lepidii new amine D, a semen lepidii new amine E and a preparation method and application thereof and effectively solves the problems of extracting the semen lepidii new amine D and the semen lepidii new amine E from semen lepidii and preparing medicines for treating cardiac muscle cell H9c2 injure from the semen lepidii new amine D and the semen lepidii new amine E. The preparation method comprises the following steps: plain-frying semen lepidii, adding water, decocting and extracting, carrying out alcohol precipitation on an extraction solution, concentrating liquid supernatant till the liquid supernatant is free of alcohol flavor, flowing through Dianion HP-20 column, eluting by using water and alcohol, stirring samples of an alcohol elution solution with silica gel, eluting via a mixed solution of dichloromethane and methyl alcohol, taking a fraction with dichloromethane and methyl alcohol in a ratio of 10 to 1 as a component C3, and taking a fraction with dichloromethane and methyl alcohol in a ratio of 5 to 1 as a component C4; dissolving the component C3 via methyl alcohol, enabling the component to flow through a Toyopearl HW-40 chromatographic column, eluting via methyl alcohol, dissolving 150-400mL of fraction via methyl alcohol, enabling the fraction to pass through a Sephadex LH-20 column chromatography, eluting via methyl alcohol, separating 80-150mL of fraction by using semi-preparative HPLC, collecting the fraction with retention time tR of 35.8-36.3 minutes, and drying the fraction to obtain the semen lepidii new amine E; dissolving the component C4 by using water, enabling the component to flow through an ODS column chromatography, carrying out gradient elution via water and methyl alcohol, separating a 60% methyl alcohol elution solution by using semi-preparative HPLC, collecting the fraction with retention time tR of 66.5-66.8 minutes, and drying the fraction to obtain the semen lepidii new amine D.
Description
technical field [0001] The invention relates to medicine, in particular to Tingcemine D and Tingcemine E, their preparation method and application. Background technique [0002] Tinglizi is a commonly used Chinese herbal medicine. It was first recorded in "Shen Nong's Materia Medica", and it was listed as a herbal inferior product. The medicine tastes pungent and bitter, and is very cold in nature. The "Tinglizi" included in the 2015 edition of "Chinese Pharmacopoeia" has a north-south distinction. Among them, the dry mature seeds of the cruciferous plant Lepidium apetalum Willd. .) The dry mature seeds of Webbex Prantl. are commonly called "Nan Ting Li Zi". [0003] From the research experiment, it is found that Tinglizi contains benzamide compounds, namely Tinglixinamine D and Tinglixinamine E, but how to extract these compounds from Tinglizi and effectively use them in Preparation of drugs for the treatment of cardiomyocyte H9c2 injury has not been publicly reported so ...
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