Preparation method of digital green intelligent high-purity marsdenia tenacissima component group and marsdenia tenacissima glycoside H and pharmaceutical composition thereof

A technology of vine vine glycoside and vine vine, which is applied in the field of digital, green, intelligent, high-purity vine vine glycoside and preparation of vine vine glycoside H and its pharmaceutical composition. Problems such as large loss of parts, to achieve the effects of shortening the production cycle, avoiding uneven quality, and reducing demand

Pending Publication Date: 2020-09-22
NANJING CHENXIANG MEDICAL RES +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although Tengguan vine contains more than a hundred kinds of active ingredients, the content of each component is very small, and the highest content of Tengguan glycoside H is only about 0.1%, and the water solubility of Tengguan glycosides is small. The preparation process is to use boiled alcohol Shen, the loss of effective parts is relatively large. At present, the content of active ingredients in the extract of Guanguanteng and its preparations is relatively low, and the color is relatively dark. Many, especially the quality of medicinal materials is affected by the place of origin, growth period, harvesting season, processing methods, etc. The quality of the product does not have a digital fixed dose, and it is difficult to control the uniformity of the product within a batch and the reproducibility between batches

Method used

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  • Preparation method of digital green intelligent high-purity marsdenia tenacissima component group and marsdenia tenacissima glycoside H and pharmaceutical composition thereof
  • Preparation method of digital green intelligent high-purity marsdenia tenacissima component group and marsdenia tenacissima glycoside H and pharmaceutical composition thereof
  • Preparation method of digital green intelligent high-purity marsdenia tenacissima component group and marsdenia tenacissima glycoside H and pharmaceutical composition thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation of embodiment 1 Tengguan rattan component group

[0050] 1) Extraction: Take 500g of Tengguan Teng powder, heat 4000ml of 30% ethanol solution, stir and extract quickly for 20min, centrifuge and filter while hot, heat 3000ml of 30% ethanol solution for filter residue 1, stir and extract quickly for 10min, centrifuge and filter while hot, and combine The two coarse filtrates were left to cool at room temperature for 2 hours, and filtered by intelligent cross-flow to obtain the fine filtrate. The fine filtrate is carried out to HPLC detection, and spectrogram sees figure 1 .

[0051] 2) Purification: Take the fine filtrate and pass it through the FL-2 macroporous adsorption resin column, wash it with 8BV of purified water, 8BV of 20% alcohol solution, 16BV of 30% alcohol solution, and 16BV of 40% alcohol solution until colorless or almost colorless, 3BV Elute with 50% ethanol solution, the flow rate is 1-2BV / h, collect the ethanol eluate that meets the t...

Embodiment 2

[0052] Example 2 The preparation of glucoside H

[0053] Take an appropriate amount of the above-mentioned preliminarily purified vine component group solution, pass through a C18 alkyl bonded silica gel column, wash and / or elute with 46% acetonitrile solution, collect vine glycoside H (area normalized Purity≧98.5%) eluate, acetonitrile is recovered under reduced pressure at 45°C to obtain a glucoside H solution, which is spray-dried under negative pressure to obtain an off-white powdered glucoside H with a purity of 99.22% and a yield of 95.59%. Chrysanthemum glucoside H is detected by HPLC according to the method of Example 1, and the spectrogram is shown in image 3 , the same method was used to detect the reference substance of guanvine glucoside H by HPLC, and the spectrum is shown in Figure 4 . After comparison with the spectrum of the reference substance, the sample is consistent with the reference substance, and the color is the same.

Embodiment 3

[0054] Example 3 The preparation of the active ingredient group of Tengguanteng

[0055] 1) Extraction Take 10kg of Tengguan rattan powder, heat 80kg of 30% ethanol solution, stir and extract quickly for 20min, centrifugally filter while hot, heat 60kg of 30% ethanol aqueous solution for filter residue 1, stir and extract quickly for 10min, centrifugally filter while hot, combine the two The crude filtrate was shaken and filtered for the first time, left to cool at room temperature for 2 hours, and filtered through intelligent cross-flow to obtain the fine filtrate.

[0056] 2) Purification: Take the fine filtrate and pass it through the FL-2 macroporous adsorption resin column, wash it with 8BV of purified water, 8BV of 20% alcohol solution, 16BV of 30% alcohol solution, and 16BV of 40% alcohol solution until colorless or almost colorless, 3BV 50% ethanol solution elution, flow rate 1-2BV / h, collect the eluate that meets the target requirements according to the set technical ...

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Abstract

The invention provides a preparation method of a digital green intelligent high-purity marsdenia tenacissima component group and marsdenia tenacissima glycoside H and a pharmaceutical composition thereof, and belongs to the technical field of traditional Chinese medicine preparation. The preparation method comprises the following steps: taking, stirring and extracting marsdenia tenacissima middlepowder with a 30% alcohol solution; carrying out throwing filtration and intelligent cross-flow filtration; passing through a macroporous adsorption resin column; performing gradient washing with an 8-16BV 0-50% alcohol solution; eluting with a 3BV 50%-60% alcohol solution; collecting target marsdenia tenacissima component group eluent, recovering alcohol until the alcohol content is 15%, passingthrough a macroporous resin column for enrichment or spray drying to obtain marsdenia tenacissima component groups, or passing through a C18 alkyl bonded silica gel column, washing and eluting with 46% acetonitrile solution, collecting target interval eluent, recovering acetonitrile until the target interval eluent is exhausted, and spray drying to obtain marsdenia tenacissima glucoside H. The method has the advantages of simple operation, energy saving, emission reduction, intelligent on-line control of the whole process, stable and controllable product quality, realization of digitization, greenization and intelligentization, and suitableness for industrial production of traditional Chinese medicines.

Description

technical field [0001] The invention provides a preparation method of digitized, green, intelligent, high-purity vine vine component group and vine glycoside H, a pharmaceutical composition and its application. Background technique [0002] Tongguan vine is the dry cane of Marsdenia tenacissima (Roxb) Wight et Arn, a plant of the genus Marsdenia tenacissima (Roxb) Wight et Arn, also known as black bone vine, Tongguangsan, Tongtiansan, and Tongguansan. It is widely distributed in tropical and subtropical regions of Asia. The 1977, 2010, and 2015 editions of "The Pharmacopoeia of the People's Republic of China" were recorded under the name "Tengguan Teng". Tong Guan Teng, bitter in taste and slightly sweet, has the effects of anti-inflammatory and pain-relieving, heat-clearing and detoxifying, relieving cough and relieving asthma. Modern pharmacology and clinical trials have proved that Tongguanteng has the functions of anti-cancer, lowering blood pressure, and regulating imm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00A61K31/7048A61P35/00A61P35/02A61P11/06A61P11/10A61P11/14A61P29/00
CPCC07J71/0005A61K31/7048A61P35/00A61P35/02A61P11/06A61P11/10A61P11/14A61P29/00
Inventor 邢宸吴祖栋邢为藩
Owner NANJING CHENXIANG MEDICAL RES
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