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Preparation method and application of chemical components in Gualoupi injection

A technology of Trichosanthes rind injection and chemical composition, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve limitations and other problems, and achieve the effect of stable and uniform compound content

Active Publication Date: 2017-12-26
SPH NO 1 BIOCHEM & PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing literature on the chemical composition of Gualoupi Injection is still limited to the amino acid composition

Method used

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  • Preparation method and application of chemical components in Gualoupi injection
  • Preparation method and application of chemical components in Gualoupi injection
  • Preparation method and application of chemical components in Gualoupi injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Preparation of Gualoupi Injection Stock Solution

[0048]After cutting 5 kg of Trichosanthes rind into small pieces, add 25 L of deionized water, extract under normal pressure for 3 times under reflux, each time for 2 hours, and combine the extracts. Concentrate the obtained extract to 10 kg, add 90% ethanol while it is hot until the alcohol content is 75%, and place it at room temperature for 48 hours to allow it to fully precipitate. Filter the supernatant. The resulting supernatant was concentrated to 5 L, and ethanol was recovered. 5L concentrated liquid on 732 type cation exchange resin column (the resin is purchased from the strong acidic cation resin of Shanghai Resin Factory, packed into a chromatographic column with a diameter of 40cm and a length of 1.5m, pre-washed with 25L distilled water, and the flow rate is 500mL / min), the adsorption is effective components, discard the effluent, wash with 50L deionized water after sample loading, and then use...

Embodiment 2

[0050] Example 2 Column chromatography enrichment target compound

[0051] Take 100g of Gualoupi injection extract, mix it with 200g of 100-200 mesh silica gel purchased from Qingdao Ocean Chemical Co., Ltd., and take another 1.5kg of Qingdao Ocean Chemical Co., Ltd.’s 100-200 mesh silica gel to pack the column. The specification of the silica gel column is 12 cm in diameter and 1.0 m in length. Analytical methanol and dichloromethane from Sinopharm Chemical Reagent Co., Ltd. were selected as eluents for column chromatography elution.

[0052] Methanol: dichloromethane (volume ratio) = 1:3 and 4 column volumes were eluted first, and the eluent was discarded. Change to methanol: dichloromethane (volume ratio) = 1:1 for elution, collect the eluate, and use rutin as a reference substance to monitor with thin-layer chromatography. After the spots displayed by rutin become lighter, the collection is ended. A total of 6 L of the eluent was collected, and concentrated under reduced...

Embodiment 3

[0053] Example 3 Column Chromatography Enrichment Target Compound

[0054] Take 150g of Trichosanthes Injection Extract, mix the sample with 200g of 100-200 mesh silica gel purchased from Qingdao Ocean Chemical Co., Ltd., and take another 1.5kg of 100-200 mesh silica gel from Qingdao Ocean Chemical Co., Ltd. to pack the column. The silica gel column specification is 12 cm in diameter and 1.0 m in length. Analytical methanol and dichloromethane from Sinopharm Reagents were selected as eluents for column chromatography elution.

[0055] Methanol: dichloromethane (volume ratio) = 1:3, eluted for 5 column volumes first, and discarded the eluent. Replace with methanol: dichloromethane = 1:1 (volume ratio), collect the eluate, and use rutin as a reference substance to monitor with thin-layer chromatography. After the spots displayed by rutin become lighter, stop collecting and collect 8 L of the eluent was concentrated under reduced pressure to remove the solvent in the collected ...

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Abstract

The invention discloses a preparation method of chemical components in a trichosanthes kirilowii Maxim injection and an application of the chemical components. The preparation method comprises steps as follows: (1), a trichosanthes kirilowii Maxim injection concentrate and silica gel are mixed and stirred, a mixture is subjected to normal-phase silica-gel column chromatography, is eluted by utilizing a mixed solution of methyl alcohol and dichloromethane in a volume ratio being 1: (3-4) as an eluent, and then is eluted by utilizing a mixed solution of methyl alcohol and dichloromethane in a volume ratio being 1: (1-1.5) as the eluent, an eluate is collected and subjected to reduced-pressure concentration, and a chromatographic product is obtained; (2), the chromatographic product and methyl alcohol are mixed, the mixture is stirred at the room temperature, is cooled to 0-4 DEG C and then is filtered, a filtrate a is obtained, a filter cake and water are uniformly mixed and then are filtered, a filtrate b is obtained, the filtrate a and the filtrate b are combined and concentrated, and the concentrate is obtained; (3), the concentrate is purified through high-pressure preparative liquid chromatography, and adenosine is obtained. The content of a compound prepared with the preparation method is stable and homogeneous, and the compound can be taken as an index for quality control on the trichosanthes kirilowii Maxim injection.

Description

technical field [0001] The invention relates to the field of medicines, in particular to a preparation method and application of chemical components in Gualoupi injection. Background technique [0002] Gualou (Latin scientific name: Trichosantheskirilowii Maxim.) root (Chinese medicine name Tianhuafen), pulp (Chinese medicine name Trichosanthes), peel (Chinese medicine name Trichosanthes skin), seeds (Chinese medicine name Trichosanthes kernel) are all famous Chinese medicines. Among them, Gualoupi is made into injection (Gualoupi Injection, Shanghai Shanghai First Biochemical Pharmaceutical Co., Ltd.), which is widely used in China for angina pectoris and coronary heart disease due to its excellent quality and curative effect. [0003] As a common traditional Chinese medicine, the chemical composition of Trichosanthes peel is very complex, and its real active ingredients have not been made clear so far. Some of the chemical constituents of Trichosanthes peel have been discl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/167C07H1/06C07H17/07G01N30/02
CPCC07H1/06C07H17/07C07H19/167G01N30/02G01N2030/027
Inventor 袁永雷陈辰黄臻辉
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD