Preparation method of high-purity sennoside and sennoside or derivative prepared by same

A kind of sennoside, high-purity technology, applied in the field of preparation of sennoside or derivatives, high-purity sennoside, can solve the problems of easy decomposition, troublesome decoction decoction, complicated operation procedures, etc., and achieves easy scale-up production , The cost of the solution is high, and the separation effect is good.

Pending Publication Date: 2021-12-31
YANGZHOU AIDEA BIOTECH
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  • Summary
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  • Application Information

AI Technical Summary

Problems solved by technology

Gu Yan et al. used macroporous resins to purify sennosides. The content of sennosides prepared by this method reached 50%, and the content of total sennosides reached more than 50%. Degradation, and due to the poor stability of sennoside, it is easy to decompose when exposed to heat and light, and transform into monoanthrone components. It is difficult to efficiently extract this component by conventional extraction and macroporous adsorption chromatography.
Taking the content of sennoside A as an index, Zhang Yang et al. studied the process conditions for extracting dianthrone in senna leaves, and obtained a product with a total sennoside content of 47.2%, with a yield of 2.93%. However, this method uses the organic solvent n-butyl Alcohol and ethanol, high cost and not environmentally friendly
Patent CN105254689A discloses a sennoside A.B salt compound and its preparation method and application. Senna leaves are used as raw materials to obtain a high-purity active ingredient sennoside A.B salt compound with a purity of 80% to 90%. , the same steps of this method are relatively cumbersome, and the last step of purification process uses acetone, methanol and other highly toxic organic solvents
[0003] In the prior art, senna traditional Chinese medicine is usually taken in the form of decoction or granules, and the decoction of the decoction is cumbersome, backward, and the dosage is large, and it cannot play a first aid role.
Current sennoside purification methods do not meet existing requirements

Method used

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  • Preparation method of high-purity sennoside and sennoside or derivative prepared by same
  • Preparation method of high-purity sennoside and sennoside or derivative prepared by same
  • Preparation method of high-purity sennoside and sennoside or derivative prepared by same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1: (1) Medicinal material extraction: get 100g senna medicinal material (wherein sennoside A+sennoside B content is 1.25%) add 8 times (g / mL) 0.1% sodium bicarbonate solution stirring extraction 60min after filtering , leave the supernatant as the extract (extract sampling test), add 6mol / L HCl to adjust the pH to 3.0, remove some impurities, filter and leave the supernatant, add sodium chloride to adjust the conductivity to 20mS / cm, add 5mol / L L NaOH adjusts pH to be 3.5, obtains sample solution (acid adjustment sample solution sampling detection);

[0047] (2) Ion-exchange column chromatography: 300 mL of A451 (ZG A451 type, Hangzhou Zhengguang Resin Co., Ltd.) macroporous weakly basic anion-exchange chromatography column is pre-installed, and the column is equilibrated 5 times with equilibrium solution A at a linear velocity of 60 cm / h Volume, balance liquid A is 0.02mol / L glycine buffer solution, contains 0.2mol / L NaCl, pH is 3.5, and conductivity is 23mS...

Embodiment 2

[0054] Embodiment 2: (1) medicinal material extraction: get 100g senna medicinal material (wherein sennoside A+sennoside B content is 1.23%) add 10 times (g / mL) 0.25% sodium bicarbonate solution and stir to extract 90min after filtering , leave the supernatant as the extract (extract sample detection), add glacial acetic acid to adjust the pH to 4.5, filter and leave the supernatant, add sodium chloride to adjust the conductance to 15mS / cm, add 5mol / L NaOH to adjust the pH to 7.0, Obtain the sample solution (acid adjustment sample solution sampling detection);

[0055] (2) Ion-exchange column chromatography: 300mL macroporous weakly basic anion-exchange chromatography column of A351 type (ZG A351 type, Hangzhou Zhengguang Resin Co., Ltd.) is pre-installed, and the column is equilibrated 5 times with equilibrium solution A at a linear velocity of 60cm / h Volume, balance solution A is 0.02mol / L phosphate buffer, containing 0.15mol / L NaCl, pH is 7.0, conductivity is 18mS / cm, then ...

Embodiment 3

[0063] Embodiment 3: (1) medicinal material extraction: get 1000g senna medicinal material (wherein sennoside A+sennoside B content is 1.15%), add 10 times (g / mL) 0.25% sodium bicarbonate solution and stir to extract 120min after filtration , leave the supernatant as the extract (extract sample detection), add 6mol / L HCl to adjust the pH to 5.5, filter and leave the supernatant, add sodium chloride to adjust the conductivity to 7mS / cm, add 5mol / L NaOH to adjust the pH to 10.0, to obtain the sample solution (acid adjustment sample solution sampling detection);

[0064] (2) Ion-exchange column chromatography: 1500mL macroporous weakly basic anion-exchange chromatography column of A313 type (ZG A313 type, Hangzhou Zhengguang Resin Co., Ltd.) is pre-installed, and the column is equilibrated 5 times with equilibrium solution A at a linear velocity of 60cm / h Volume, balance liquid A is 0.2mol / L sodium bicarbonate buffer solution, contains 0.1mol / L NaCl, pH is 10.0, and conductivity ...

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Abstract

The invention discloses a preparation method of high-purity sennoside and sennoside or derivatives prepared by the preparation method. The preparation method comprises the following steps: (1) extracting medicinal materials; (2) ion exchange column chromatography: balancing an ion exchange column by using equilibrium liquid A which is 3-5 times of the column volume; loading the acid-regulated supernate obtained in the step (1) onto a chromatographic column, rebalancing by using equilibrium liquid A with the volume 3-5 times that of the column, and eluting by using eluent B with the volume 3-5 times that of the column to obtain eluent; (3) macroporous adsorption column chromatography: adjusting the pH value of the eluent obtained in the step (2) to 3.5-8.0, then loading the eluent to a macroporous adsorption chromatographic column, and eluting with an eluent E with the volume 3-5 times that of the column to obtain the eluent; and (4) carrying out low-temperature precipitation and solid-liquid separation on the eluent obtained in the step (3) to obtain an extract of the sennoside A / B compound. The sennoside is purified by using the macroporous adsorption chromatographic column and the ion exchange column chromatography, and the obtained sennoside extract is high in purity, low in cost and more environment-friendly.

Description

technical field [0001] The invention relates to the technical field of plant extraction, in particular to a method for preparing high-purity sennoside and the prepared sennoside or derivative thereof. Background technique [0002] The main active ingredients in Folium sennae are anthraquinone derivatives. Among the anthraquinone derivatives, the dianthrone derivatives sennosides A, B, C, and D have stronger laxative effect and irritation than other anthraquinone-containing laxatives, and have little toxicity when taken orally, so they are commonly used in clinic For acute constipation. Dianthrone compounds are formed by connecting two molecules of anthrone C-C, wherein sennosides A and B, sennosides C and D are stereoisomers of each other. Sennosides have inhibitory effects on Streptococcus pneumoniae, Klebsiella pneumoniae and Staphylococcus aureus. In addition, sennosides also have insulin-sensitizing and α-glucoamylase inhibitory effects. Gu Yan et al. used macroporou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/244C07H1/00C07H1/08
CPCC07H15/244C07H1/00C07H1/08
Inventor 吴佳佳池玉梅谈悦杨兴乐王建强袁玉俞恒傅和亮
Owner YANGZHOU AIDEA BIOTECH
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