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Purification method for lobule protopine

A purification method and a technology for phyllophyllin, which are applied in the field of extracting and purifying phyllophyllin, can solve the problems of low yield, large sample loss and high cost, and achieve the effects of high product purity, improved extraction rate and easy dissolution.

Inactive Publication Date: 2013-01-09
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has large sample loss, low yield and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take the dried leaves of the small-leaf fragrant tea, crush them through a 60-mesh sieve, weigh 5kg, add 15L of cellulase aqueous solution of pH4.2 (add 2.2g of cellulase per kilogram of crude drug) to soak for half an hour, and then enzymatically hydrolyze in a water bath at 42°C 3 hours, fully stirred, filtered, and the filter residue was extracted with 80% ethanol with 5 times the weight of the medicinal materials under reflux for 1 hour, extracted 3 times, combined the extracts, concentrated under reduced pressure to obtain the extract, heated the extract to disperse, added XAD -16 macroporous adsorption resin column, first take 3BV10% ethanol to elute impurities, then take 4BV70% ethanol to elute active ingredients, recover ethanol under reduced pressure to obtain crude extract, extract with equal volume of chloroform, extract continuously 4 times, combine The extract is concentrated and then subjected to silica gel column chromatography (silica gel particle size is...

Embodiment 2

[0021] Take the dried leaves of the small-leaf fragrant tea, crush them through a 60-mesh sieve, weigh 5kg, add 15L of cellulase aqueous solution of pH 4.2 (3.1g of cellulase per kilogram of crude drug) to soak for half an hour, and then enzymatically hydrolyze in a water bath at 44°C 2 hours, fully stirred, filtered, the filter residue was extracted with 90% ethanol with 6 times the weight of the medicinal materials under reflux for 1 hour, extracted twice, the extracts were combined, concentrated under reduced pressure to obtain the extract, the extract was dispersed by heating water, and added AB -8 macroporous adsorption resin column, first take 4BV20% ethanol to elute impurities, then take 4BV90% ethanol to elute active ingredients, recover ethanol under reduced pressure to obtain crude extract, extract with equal volume of chloroform, extract continuously 4 times, combine The extract is concentrated and then subjected to silica gel column chromatography (silica gel partic...

Embodiment 3

[0023] Take the dried leaves of the small-leaf fragrant tea and pulverize through a 60-mesh sieve, weigh 5kg, add 15L of cellulase aqueous solution of pH4.2 (add 1.8g of cellulase and pectinase mixed compound enzyme, cellulase and pectin per kilogram of crude Enzyme (mass ratio: 1:1) was soaked for half an hour, then enzymolyzed in a water bath at 50°C for 5 hours, fully stirred, filtered, and the filter residue was heated and refluxed with 90% ethanol 5 times the weight of the medicinal materials for 1 hour, and 2 The second time, combine the extracts, concentrate under reduced pressure to obtain the extract, heat the extract to disperse in water, add XDA-8 macroporous adsorption resin column, first take 3BV10% ethanol to elute impurities, then take 6BV90% ethanol to elute active ingredients, and decompress Recover ethanol to obtain the crude extract, extract with chloroform of equal volume, and extract continuously for 4 times, combine the extracts, concentrate the extracts a...

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PUM

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Abstract

The invention discloses a purification method for lobule protopine. The method includes: (1), taking raw materials isodon parvifolius dried leaves, subjecting to crushing treatment, soaking by enzyme solution, performing water bath enzymolysis and fully stirring; (2), filtering enzymatic hydrolysate, taking filter residue for extraction for 2-3 times with ethanol water in amount of 5-10 folds, merging extraction liquid, and decompressing and concentrating to obtain extract; (3) subjecting the extract to go through a macroporous adsorption resin column, eluting with alcohol-water mixed solution, and collecting eluted liquid; and (4), depressing the eluted liquid to recycle ethanol, extracting with chloroform, placing extraction liquid after concentration onto a silica column, performing gradient elution with ethyl acetate-ethanol, adopting TLC (thin layer chromatography) for tracking and monitoring, collecting lobule protopine fraction, decompressing and concentrating, cooling and drying to obtain the product. The purification method for lobule protopine is simple in operation, high in yield of obtained products, low in cost and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of plant extraction, and relates to a method for extracting and purifying patinin from dried leaves of japonica. Background technique [0002] Small-leaf caraway Isodon parvifolia (Batalin) Hara is a plant of the genus Batalinaceae, which is mainly distributed in Sichuan Province of my country. In 1990, Guo Yuewei et al. first isolated lobectin from the leaves of the lobular tea, and preliminary pharmacological studies showed that lobectin has a certain inhibitory effect on human liver cancer cell line QGY-7703. The method adopted by Guo Yuewei and others is to extract with 95% ethanol, decolorize with activated carbon with 2% crude drug amount, and process the alcoholic extract by conventional methods, extract with ethyl acetate several times, recover, separate on silica gel column, and separate by chloroform-acetone gradient elution to obtain Leptin. This method has large sample loss, low yield and hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/68C07C51/42
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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