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Method for preparing thalictricoside

A technique of tangeloside and Metten, which is applied in the field of preparation of tangeloside, can solve the problems of large amount of organic solvent used, long separation process time, large sample loss, etc., and achieves saving of organic solvent, high recovery rate, and high product quality. high purity effect

Inactive Publication Date: 2011-11-02
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, traditional column chromatography is mainly used to separate oriental tangeloside from geranium seeds. For example, Niufeng is extracted with 5 times the amount of 95% ethanol, the extract is concentrated, extracted with ethyl acetate and n-butanol respectively, and then subjected to AB-8 Macroporous adsorption resin column separation, collecting 30% ethanol eluting part, concentrating, repeating Sephadex LH-20, eluting with methanol-water (1:1), removing pigment, methanol recrystallization to obtain oriental tangelin, this method separates The process takes a long time, the operation is cumbersome, the sample loss is large, and the amount of organic solvent used is large
At present, there is no relevant research report on the application of high-speed countercurrent chromatography technology to the separation of tangelin in tiankui seeds

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A. Pulverize geranium seeds through an 80-mesh standard sieve, put 2kg into a small stainless steel extraction tank, add 20L deionized water for ultrasonic extraction for 1 hour, release the filtrate, then add 20L deionized water to extract twice, and combine the three extracts, Add 100 g of activated carbon to reflux for decolorization for 0.5 hour, filter out the activated carbon, and concentrate under reduced pressure to obtain a precipitate.

[0016] B. Select n-butanol-ethyl acetate-methanol-0.5% ammonia water in a volume ratio of 3:4:4:8 and put the above solvent components in a separatory funnel, shake well and then let stand to separate layers. After the two-phase solvent is balanced, separate the upper phase and the lower phase, take the upper phase as the stationary phase, and the lower phase as the mobile phase, use a semi-preparative high-speed countercurrent chromatograph with a column volume of 260ml, weigh 300mg of the precipitate and dissolve it in 100ml ...

Embodiment 2

[0019] A. Crush geranium seeds through a 60-mesh standard sieve, put 2kg into a small stainless steel extraction tank, add 30L deionized water to heat and reflux for extraction for 2 hours, release the filtrate, then add 30L deionized water to extract twice, and combine the three extracts , Add 70g of activated carbon to reflux for decolorization for 1 hour, filter out the activated carbon, and concentrate under reduced pressure to obtain a precipitate.

[0020] B. Select isobutanol-ethyl acetate-methanol-0.1% ammonia water in a volume ratio of 5:3:2:7 and put the above solvent components in a separatory funnel, shake well and let stand to separate layers. After the two-phase solvent is balanced, separate the upper phase and the lower phase, take the upper phase as the stationary phase, and the lower phase as the mobile phase, use a semi-preparative high-speed countercurrent chromatograph with a column volume of 200ml, weigh 300mg of the precipitate and dissolve it in 100ml Ob...

Embodiment 3

[0023] A. Grind geranium seeds through an 80-mesh standard sieve, put 2kg into a small stainless steel extraction tank, add 16L deionized water for ultrasonic extraction for 2 hours, release the filtrate, add 16L deionized water for extraction once, and combine the two extracts, Add 80 g of activated carbon to reflux for decolorization for 0.5 hour, filter out the activated carbon, and concentrate under reduced pressure to obtain a precipitate.

[0024] B. Select n-butanol-ethyl acetate-methanol-0.5% ammonia water in a volume ratio of 4:3:4:6 and place the above solvent components in a separatory funnel, shake well and let stand to separate layers. After the two-phase solvent is balanced, separate the upper phase and the lower phase, take the upper phase as the stationary phase, and the lower phase as the mobile phase, use a semi-preparative high-speed countercurrent chromatograph with a column volume of 240ml, weigh 300mg of the precipitate and dissolve it in 100ml Obtain sam...

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Abstract

The invention belongs to the field of natural organic chemistry, and relates to a method for preparing thalictricoside. The method comprises the following two steps of: 1, preparing crude extract of muskroot-like semiaquilegia root, namely taking coarse powder of a muskroot-like semiaquilegia root material, extracting the coarse powder for 1 to 2 hours by using deionized water in an amount which is 8 to 15 times weight (V / W) of the coarse powder, adding active carbon into the extract to decolorize the extract, and concentrating the extract to obtain sediment; and 2, separating the sediment by using high-speed countercurrent chromatography to prepare a target compound of the thalictricoside, and performing separation for two times to obtain high-purity thalictricoside. According to the method, a large amount of organic solvent can be saved, the separation process is short, and the thalictricoside has high purity and can be directly used for chromatography standard samples or commerce and the like.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry and relates to a preparation method of oriental tangeloside. Background technique: [0002] Tiankuizi is also known as purple-backed Tiankui root, millennium rat feces ("Compendium Supplements"), etc., the roots are used as medicine, sweet, bitter, cold in nature, and slightly poisonous; it has the effects of clearing heat and detoxification, reducing swelling and dispelling stagnation; used for scrofula Diseases such as boils, bloated, boils, bruises, poisonous snake bites. After research, geranium seed has inhibitory effect on Staphylococcus aureus; clinically, geranium seed or its compound is used to treat acute soft tissue injury, bone and joint tuberculosis, acute mastitis, uterine fibroids, primary liver cancer, gastric cancer, etc. Oriental tangeloside is a nitrophenol glycoside component in Tiankuizi. It is relatively rare in general plants, but it has the highest amount in gera...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/203C07H1/08
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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