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Novel compound and separation method thereof

A separation method and compound technology, applied in the direction of steroids, organic chemistry, drug combination, etc.

Active Publication Date: 2009-07-01
BEIJING WBL PEKING UNIV BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After searching SciFinder ("American Chemical Abstracts (CA) Network Database", 1907-2007.9), MEDLINE CD-ROM ("American General Medical Literature CD-ROM Database", 1966-2007.6), PubMed ("World Medical Literature Database", 2007 -2007.9) and "Chinese Biomedical Literature Database" (CBMdisc, 1978-2007.6), "Chinese Biomedical Journal Literature Database" (CMCC, 1994-2007.9), Chinese Journal Full-text Database (CNKI, 1994-2007.9), there are no domestic and foreign See the report of new compounds in Xuezhikang Capsules

Method used

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  • Novel compound and separation method thereof
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Examples

Experimental program
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Effect test

experiment example 1

[0019] Experimental example 1 HMG-CoA reductase inhibitory activity test

[0020] The new compound 3, 16, 20, 22, 23, 25-hexahydroxyergoster obtained in Example 1 was dissolved in 75% ethanol, and the concentration was 2 mg / ml; the total volume in the assay system was 200 μl, each component Concentrations are: potassium chloride 200mM, potassium dihydrogen phosphate 160mM, ethylenediaminetetraacetic acid 4mM, dithiothreitol 10mM, two substrates nicotinamide adenine dinucleotide and 3-hydroxy-3-methylpentane The concentration of diacyl-CoA is 200 μM and 50 μM, pH6.8, add 20 μL of enzyme, add 5 μl of enzyme inhibitor, add 5 μl of 75% ethanol in the control group, and detect OD on a Versamax microplate reader at 37 °C 340 dynamic changes. By detecting OD 340 The speed of decline (indicated by slope value) within 5 minutes was used to evaluate the strength of HMG-CoA reductase activity, and then to evaluate the strength of inhibitory activity of enzyme inhibitors. The results ar...

Embodiment 1

[0026] Take 2000g of the contents of Xuezhikang capsules, and use petroleum ether, chloroform, and methanol, which are 4 times the weight of the contents of Xuezhikang capsules, as solvents for ultrasonic extraction. Each solvent is ultrasonically extracted 3 times for 30 minutes each time, and the extracts are combined to recover the solvent. , take petroleum ether part P, chloroform part C, methanol part M;

[0027] Take 250 g of part C and apply it to silica gel column chromatography, and use chloroform-methanol gradient elution to obtain pure chloroform eluted fraction C-I, 95:5 chloroform-methanol eluted fraction C-II, and 90:10 chloroform-methanol eluted fraction C- III, pure methanol elution part C-IV;

[0028] Part C-III was eluted with 90:10, 80:20, 70:30, 50:50 gradients of chloroform-methanol, and the part eluted with 80:20 chloroform-methanol was subjected to repeated silica gel column chromatography to obtain new compounds Crude product 0.047g; using C-18 alkyl b...

Embodiment 2

[0030] Take 1500g of the contents of Xuezhikang capsules, and use petroleum ether, chloroform, and methanol, which are 6 times the weight of the contents of Xuezhikang capsules, as solvents for ultrasonic extraction. Each solvent is ultrasonically extracted 3 times, each time for 20 minutes, and the extracts are combined to recover the solvent. , take petroleum ether part P, chloroform part C, methanol part M;

[0031] Take 300 g of part C and apply it to silica gel column chromatography, and use chloroform-methanol gradient elution to obtain pure chloroform elution fraction C-I, 95:5 chloroform-methanol elution fraction C-II, 90:10 chloroform-methanol elution fraction C- III, pure methanol elution part C-IV;

[0032] Part C-III was eluted with 90:10, 80:20, 70:30, 50:50 gradients of chloroform-methanol, and the part eluted with 80:20 chloroform-methanol was subjected to repeated silica gel column chromatography to obtain new compounds Crude product 0.042g; using C-18 alkyl b...

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Abstract

The invention discloses a new compound of 3,16,20,22,23,25-hexahydroxy ergostane and a separation method thereof. The chemical structural formula of the compound of 3,16,20,22,23,25-hexahydroxy ergostane is shown by the right formula. Experimental results show that the compound of 3,16,20,22,23,25-hexahydroxy ergostane has the HMG-CoA reductase inhibiting effect.

Description

technical field [0001] The present invention relates to a novel compound and a separation method thereof, in particular to a novel compound 3, 16, 20, 22, 23, 25-hexahydroxyergoster and a separation method thereof. Background technique [0002] Xuezhikang capsules are rich in a series of natural statins, including monacolin K (lovastatin), monacolin K sodium hydroxy acid (acid form, ring-opening form), monacolin K lactone dehydrate, monacolin L, monacolin J lactone and Dehydrated substances, etc., most of the ingredients have lipid-lowering activity. Xuezhikang capsules also contain isoflavones, sterols, 20 kinds of amino acids, unsaturated fatty acids and various trace elements. The isoflavone components mainly include genistein, daidzein, and glycitein, and the free isoflavone content is about 0.045%. The content of sterols in Xuezhikang Capsules is 0.3%, including ergosterol, stigmasterol and sitosterol. The chemical name of ergosterol is 24β-methylcholesterol-5,7en-3β...

Claims

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Application Information

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IPC IPC(8): C07J9/00A61K31/56A61P43/00
Inventor 段震文郭树仁何大林马学敏
Owner BEIJING WBL PEKING UNIV BIOTECH
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