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Method for simultaneously preparing pedunculoside and syringin

A technology of syringin and syringin, which is applied in chemical instruments and methods, preparation of sugar derivatives, steroids, etc., can solve the problem of loss of syringin, high cost, loss of syringin and syringin, etc. problem, to achieve the effect of simple and easy method, high product yield and short cycle

Active Publication Date: 2012-08-22
INST OF CHINESE MATERIA MEDICA CHINA ACAD OF CHINESE MEDICAL SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional purification process is long and the loss of the target compound is large. Multiple silica gel column chromatography is used. The operation steps are numerous and the eluent is mainly toxic and expensive reagents such as chloroform, acetone, and ethyl acetate.
The Chinese patent "Preparation Method and Application of Pelicin" (Publication No. CN101033245) adopts the traditional method of extracting and rescuing Bing with alcohol, only obtains Pelagin with a purity of 98%, and loses a large amount of syringin
[0006] To sum up, in the process of extracting and separating pelicin and syringin, there are common problems such as the loss of pelicin and lilac, long purification process, high toxicity of solvent residue, and high cost.

Method used

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  • Method for simultaneously preparing pedunculoside and syringin
  • Method for simultaneously preparing pedunculoside and syringin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Take 1Kg of dried Bingying, add 12 times the amount (12L) of 50% ethanol aqueous solution for reflux extraction once, the extraction time is 1h, collect the extract, recover ethanol, concentrate under reduced pressure to 10L, centrifuge, and pass the supernatant through SP825 macroporous adsorption resin (5L) (ID10cm * H70cm) after pretreatment, after sample loading finishes, first use 3 times of resin volume, volume fraction is 20% ethanol aqueous solution elution, then with 4 times of resin volume, volume fraction is Eluted with 50% ethanol aqueous solution, detected by HPLC method (chromatographic conditions: Agilent1200 high performance liquid chromatograph, Shiseido UG120-C18 chromatographic column (4.6 × 150mm, 5 μ m), mobile phase is acetonitrile and water, gradient elution program is 0- 10min, 10% acetonitrile; 10-20min, 10%-40% acetonitrile; 20-30min, 40% acetonitrile; detection wavelength is 210nm, flow rate is 1mL / min, column temperature is 25°C), syringin is ...

Embodiment 2

[0042] Take 1Kg of dried Bingying, add 12 times the volume (12L) of 50% ethanol aqueous solution to reflux and extract twice, extract for 1 hour each time, combine the two extracts, recover ethanol, concentrate under reduced pressure to 12L, centrifuge, and remove the supernatant solution through the pretreated SP825 macroporous adsorption resin (5L) (ID10cm×H70cm), after loading the sample, first use 2 times the resin volume, the volume fraction is 10% ethanol aqueous solution to elute, and then use 3 times the resin volume, volume The fraction is eluted with 40% ethanol aqueous solution, and detected by HPLC method, syringin is mainly concentrated in the part eluted with 10% ethanol, and pelicin is mainly concentrated in the part eluted with 40% ethanol.

[0043] The 10% ethanol eluted part was concentrated and dried to obtain crude syringin. Dissolve the crude product in methanol aqueous solution with a volume fraction of 10%, pass through the treated open ODS chromatograph...

Embodiment 3

[0046] Take 1Kg of dried Bingying, add 12 times the amount (12L) with a volume fraction of 50% ethanol aqueous solution to reflux and extract 3 times, each time for 1h, combine the 3 extracts, recover ethanol, concentrate under reduced pressure to 8L, centrifuge, and remove the supernatant solution through the pretreated HP20 macroporous adsorption resin (5L) (ID10cm×H70cm), after loading the sample, first use 4 times the resin volume, the volume fraction is 30% ethanol aqueous solution to elute, and then use 5 times the resin volume, volume Fractions are eluted with 60% ethanol aqueous solution, and detected by HPLC method, syringin is mainly concentrated in the part eluted with 30% ethanol, and pelicin is mainly concentrated in the part eluted with 60% ethanol.

[0047] The 30% ethanol eluted part was concentrated and dried to obtain crude syringin. Dissolve the crude product in methanol, place it in a water bath at 60°C to make it a supersaturated solution, then let it stan...

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Abstract

The invention discloses a method for simultaneously preparing high-purity syringin and pedunculoside. According to the method, the high-purity syringin and the high-purity pedunculoside are prepared by using holly barks as a raw material, adopting a solvent extraction method and a macromolecular resin adsorption method for extraction and separation and adopting re-crystallization, open ozone depleting substance (ODS) column chromatography or Se-phadex LH-20 column chromatography, liquid chromatography and the like. The purity of each of the syringin and the pedunculoside is over 90 percent, and the method is simple, feasible and suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for simultaneously preparing pelicin and syringin. Background technique [0002] Jiubiying is the dry bark of Ilex rotunda Thunb., a plant in the Ilex family, which was first recorded in "Lingnan Herb Collection", also known as Baimuxiang, Yangbuchi, Baichenxiang and so on. Iron holly grows in sparse forests at the foot of the mountain or beside ditches and streams, and is distributed in Jiangsu, Anhui, Zhejiang, Jiangxi, Fujian, Taiwan, Hunan, Guangdong, Guangxi, and Yunnan. It is a commonly used herbal medicine in southern my country. It has the effects of clearing away heat and detoxification, promoting dampness and relieving pain. It is often used to treat heat-damp fever, sore throat, damp-heat diarrhea, abdominal distension and pain, rheumatic arthralgia, eczema, boils, and bruises. In addition, the ethanol extraction part of Jiubingying has strong antibacterial and anti-inflammatory effects [Zhang Rongwen, Huan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00C07H15/203C07H1/08
Inventor 巢志茂王淳吴晓毅孙文谭志高刘海萍
Owner INST OF CHINESE MATERIA MEDICA CHINA ACAD OF CHINESE MEDICAL SCI
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