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The preparation method of 1,3,7,9-tetramethyluric acid

A technology of tetramethyluric acid and ethyl acetate, applied in the direction of organic chemistry, can solve the problems of low sample yield, small preparation amount, large pollution, etc., and achieve the effect of retaining biological activity, large preparation amount, and high yield

Active Publication Date: 2019-02-22
UNO SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the low yield and small amount of preparation of samples by macroporous resin column chromatography, normal phase column chromatography and reverse phase column chromatography, large-scale preparation cannot be carried out, and the pollution is large, time-consuming and costly
In addition, a large amount of adsorption fillers are used in the preparation process, which easily leads to a large discount on the original biological activity of the sample, reduces the activity of the prepared 1,3,7,9-tetramethyluric acid, and reduces the production efficiency. suitable for promotional use

Method used

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  • The preparation method of 1,3,7,9-tetramethyluric acid

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Embodiment 1

[0032] A preparation method of 1,3,7,9-tetramethyluric acid in this embodiment comprises the following steps:

[0033] S1, get bitter tea extract 11.9g as the sample to be separated; Preparation volume ratio is the solvent system of ethyl acetate, n-butanol and water of 1:1.5:3, and described solvent system comprises upper stratum and lower strata, in described upper strata Add the triethylamine of 10mmol / L as stationary phase, add the hydrochloric acid of 10mmol / L in the lower layer as mobile phase, get 120mL described mobile phase and dissolve described sample to be separated, obtain the solution to be separated;

[0034] S2. Pump the stationary phase and mobile phase into the chromatographic column of high-speed countercurrent chromatography, the head end goes in, and the tail end goes out; The countercurrent chromatogram obtained by the recorder determines whether 1,3,7,9-tetramethyluric acid (appearing figure 2 The chromatogram shown shows that the fractions contain 1,3...

Embodiment 2

[0036] In this example, a method for preparing 1,3,7,9-tetramethyluric acid, the steps are similar to Example 1, the difference is that the solvent system in step S1 is ethyl acetate with a volume ratio of 1.5:0.5:1, n-butanol and water.

Embodiment 3

[0038] In this example, a method for preparing 1,3,7,9-tetramethyluric acid, the steps are similar to Example 1, the difference is that the solvent system in step S1 is ethyl acetate with a volume ratio of 0.5:2:6, n-butanol and water.

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Abstract

The invention relates to a preparation method of 1,3,7,9-tetramethyluric acid. The preparation method comprises the following steps: bitter tea extract is taken as a to-be-separated sample, ethyl acetate, n-butanol and water constitute a solvent system, the to-be-separated sample is subjected to elution separation with high-speed countercurrent chromatography, whether fractions contain 1,3,7,9-tetramethyluric acid is determined according to a countercurrent chromatography map obtained by a recorder, the fractions containing 1,3,7,9-tetramethyluric acid are collected and dried, and 1,3,7,9-tetramethyluric acid is obtained. 1,3,7,9-tetramethyluric acid prepared with the preparation method is high in purity and yield, single preparation quantity is large, sample activity is not affected, and additional pollution is avoided. Prepared 1,3,7,9-tetramethyluric acid can be applied to medicines, cosmetics, health care products and the like.

Description

technical field [0001] The invention relates to the field of extraction and separation technology of active ingredients of traditional Chinese medicines, in particular to a preparation method of 1,3,7,9-tetramethyluric acid. Background technique [0002] 1,3,7,9-Tetramethyluric acid (TC), whose structural formula is shown in formula (I), is a naturally occurring purine alkaloid, mainly present in bitter tea, and has antidepressant, sedative hypnotic and antidepressant properties. Pharmacological effects such as inflammation and analgesia. Since the content of 1,3,7,9-tetramethyluric acid in bitter tea is small, how to prepare it with high yield has attracted extensive attention. [0003] At present, most of the methods for separating 1,3,7,9-tetramethyluric acid are macroporous resin column chromatography, normal phase column chromatography and reverse phase column chromatography. Due to the low sample yield and small preparation volume of macroporous resin column chromato...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D473/14
CPCC07D473/14
Inventor 黄启吟连林生曾仑
Owner UNO SCI CO LTD
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