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Method for extracting and separating tectoridin from iris tectorum

A technology of Sichuan Shegan and Shegan glycosides, which is applied in the field of extraction of active ingredients of plants, can solve the problems of excessive waste liquid, high cost of extraction and separation, and high energy consumption, and achieve simple process flow, improved utilization value, and low total solvent consumption Effect

Active Publication Date: 2012-07-25
武汉回盛生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The target product content of the above process is high, but the chromatography efficiency is low, and the eluent needs a large amount; the concentration of the product in the eluent is generally small, and the product must be concentrated and dried, which requires a lot of energy and labor intensity ; Solvent separation and purification after elution is more difficult, not easy to recycle, more waste liquid, high cost of extraction and separation, serious pollution, seriously restricting the improvement of product quality and the reduction of product production cost
Therefore, low-cost separation methods that can be applied on an industrial scale remain a challenge

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for extracting and isolating Shegan glycosides from Sichuan Shegan, the steps are as follows:

[0022] A, take Sichuan and shoot dry, pass through 100 mesh sieves after drying and pulverizing;

[0023] B. Weigh 100g of sifted Chuanshegan, add it to 1500mL of a two-phase solvent system prepared by n-butanol and water volume ratio of 1:2 and carry out stirring and extraction. The extraction time is 1.5 hours, the stirring speed is 500rpm, and the extraction temperature is 40°C;

[0024] C. Filtration. After the obtained filtrate is layered and stable in the separatory funnel, separate the upper layer of n-butanol phase, concentrate it under reduced pressure to 40mL, and leave it overnight. There are a large amount of yellow-white precipitates. Filter and filter the residue with an equal weight 6.20 g of the off-white schiquatin crude product was obtained after washing with absolute ethanol, and the content of schiquatin in the crude product was 74.38% (detected ...

Embodiment 2

[0026] A method for extracting and isolating Shegan glycosides from Sichuan Shegan, the steps are as follows:

[0027] A, take Sichuan and shoot dry, pass through 100 mesh sieves after drying and pulverizing;

[0028] B. Weigh 100g of sifted Chuanshegan, add it to 1800mL of a two-phase solvent system prepared by n-butanol and water volume ratio of 2:1 and carry out stirring and extraction. The extraction time is 2 hours, the stirring speed is 450rpm, and the extraction temperature is 60°C;

[0029] C. Filtration. After the obtained filtrate is layered and stable in the separatory funnel, separate the upper layer of n-butanol phase, concentrate it under reduced pressure to 45mL, and leave it overnight. There are a large amount of yellow-white precipitates. Filter and filter the residue with an equal weight Washed with absolute ethanol and dried to obtain 6.19g of off-white crude product of radishes, the content of which is 75.63%; then recrystallized twice with 95v / v% ethanol ...

Embodiment 3

[0031] A method for extracting and isolating Shegan glycosides from Sichuan Shegan, the steps are as follows:

[0032] A, take Sichuan and shoot dry, pass through 80 mesh sieves after drying and pulverizing;

[0033] B. Weigh 100g of sifted Chuanshegan, add it to 1600mL of two-phase solvent system prepared by n-butanol and water volume ratio of 1:1 and carry out stirring and extraction. The extraction time is 1.5 hours, the stirring speed is 400rpm, and the extraction temperature is 55°C;

[0034] C. Filtration. After the obtained filtrate is layered and stable in the separatory funnel, separate the upper layer of n-butanol phase, concentrate it under reduced pressure to 40mL, and leave it overnight. There are a large amount of yellow-white precipitates. Filter and filter the residue with 1.5 times After washing with 50% absolute ethanol, dry it to obtain 6.47g of off-white crude product of radishes, the content of which is 78.98%; then recrystallize twice with 80v / v% methano...

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Abstract

The invention discloses a method for extracting and separating tectoridin from iris tectorum. The method comprises the following steps of: (1) taking iris tectorum, drying, crushing, and sieving through a 60-100 mesh sieve; (2) weighting the sieved iris tectorum, adding into a 15-20mL / g two-phase solvent system with a volume ratio of normal butanol to water being (1:2)-(2:1), stirring and extracting, wherein the extracting time is 1.5-5h, the stirring speed is 280-800rpm and the extracting temperature is at 25-70 DEG C; and (3) after layering and stabilizing a filtrate obtained after filtering in a liquid-separating funnel, separating a normal butanol phase, reducing pressure and concentrating to 40-50mL, overnight aging till forming a large number of yellowish white educt, filtering, washing the filter residue with less absolute ethyl alcohol, and drying so as to obtain a white tectoridin crude product, wherein the content of the tectoridin in the crude product is not less than 74%; and twice re-crystallizing by using an organic solvent, thereby obtaining a tectoridin product. The method has the advantages of simple steps, low cost, and high purity of obtained product, and the content of tectoridin after re-crystallizing is above 93%.

Description

technical field [0001] The invention relates to a method for extracting plant effective components, in particular to a method for extracting and separating Shegan glycosides from Sichuan Shegan. Background technique [0002] Chuanshegan is the dried rhizome of Iris tectorum Maxim., which is a plant of the genus Iris in the family Iridaceae. It is mainly produced in Guangzhou, Guangxi, Sichuan, Guizhou and other places in my country. It is mainly used to treat sore throat, phlegm, cough and asthma, etc. It was officially included in the 2005 edition of Pharmacopoeia of the People's Republic of China. [0003] Studies have proved that the main active ingredients in Sichuan Shegan are irisin (also known as Shegan glycoside), wild irisin, irisin, wild irisaxanthin, and second wild irisaxanthin and other isoflavones, which have anti-inflammatory and antiviral properties. , detoxification and other pharmacological activities. Existing experimental studies have shown that irisin a...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
CPCY02P20/582
Inventor 张卫元张永丹陈翠兰肖飞刘国庆周瑜
Owner 武汉回盛生物科技股份有限公司
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