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Method for producing orientin standard substance

A technology of orientin and standard products, which is applied in the field of preparation of orientin standard products, can solve the problems of insufficient purity, high cost, low yield, etc., and achieve the effect of simple process, low cost and good stability

Inactive Publication Date: 2009-03-18
黄泽奇
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current preparation method of orientin standard substance has the disadvantages of low yield, high cost and insufficient purity.

Method used

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  • Method for producing orientin standard substance
  • Method for producing orientin standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: Orientin preparation method

[0037] The medicinal material of nasturtium, add 10 times the amount of crude drug and 50% ethanol to reflux extract 3 times, each time for 2 hours, combine the extracts, recover ethanol under reduced pressure and concentrate to the extract; the extract is dissolved in methanol, loaded in dry method, passed through Column chromatography, 70:30:10 chloroform: methanol: the lower layer solution of water is the eluent, elution, TLC detection, 65:30:10 chloroform: methanol: the lower layer solution of water is the developing agent, develop, collect the The eluate of glucoside was dissolved in 80% methanol, Sephadex LH-20 column chromatography, eluted with 80% methanol; the purity of the eluate was detected by HPLC, the mobile phase was 12:88 acetonitrile-0.1% phosphoric acid water, and the detection Combine the eluate with a purity greater than 98% at a wavelength of 350 nm to obtain orientin;

Embodiment 2

[0038] Embodiment 2: Orientin preparation method

[0039] The medicinal material of nasturtium, plus 7 times the amount of crude drug, 60% ethanol reflux extraction twice, each time for 3 hours, combined extracts, recovered ethanol under reduced pressure and concentrated to a thin paste; the extract was subjected to silica gel column chromatography, 80:22:5 Chloroform: methanol: the lower layer solution of water is the eluent, elution, TLC detection, the chloroform of 70:30:10: methanol: the lower layer solution of water is the developing agent, collects the eluent containing orientin, and adds Dissolved in 70% methanol, Sephadex LH-20 column chromatography, eluted with 75% methanol; the purity of the eluent was detected by HPLC, the mobile phase: acetonitrile-0.1% phosphoric acid water was 14:82, the detection wavelength was 350nm, and the combined purity was greater than 98% of the eluate, that is, orientin.

Embodiment 3

[0040] Embodiment 3: Orientin preparation method

[0041] Tsura chinensis medicinal material, add 6 times the amount of crude drug and reflux extraction with 60% ethanol for 4 times, each time for 1 hour, combine the extracts, recover ethanol under reduced pressure and concentrate to a thin paste; the extract is subjected to silica gel column chromatography, 65:35:10 Chloroform: methanol: the lower layer solution of water is the eluent, eluting, TLC detection, the chloroform of 60:40:10: methanol: the lower layer solution of water is the developing agent, collects the eluent containing orientin, and adds Methanol dissolved, Sephadex LH-20 column chromatography, methanol elution; elution eluent was tested for purity by HPLC, mobile phase: acetonitrile-0.1% phosphoric acid water was 16:82, detection wavelength was 350nm, and the combined purity was greater than 98%. After dehydration, orientin is obtained.

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Abstract

The invention discloses a preparation method for orientin standard products, comprising the steps of: 1, adding 50% to 80% alcohol with gold lotus to process reflux extraction, decompressing, recovering and concentrating alcohol into paste; II, treating the extract paste with silica gel column chromatography, eluting and collecting the eluent containing orientin; checking the eluent via thin layer chromatography, combining the eluent containing orientin to obtain the orientin rough product of 70% to 80% purity; III, adding 70% to 100% methanol to dissolve the orientin rough product, processing Sephadex LH-20 column chromatography, eluting via 70% to 100% methanol; IV, checking the purity of Sephadex LH-20 eluent via HPLC, combining the eluent of the purity higher than 98% to obtain orientin. The preparation method has high yield and stability.

Description

technical field [0001] The invention relates to a method for preparing a standard product of a traditional Chinese medicine extract, in particular to a method for preparing a standard product of orientin. Background technique [0002] This product orientin is derived from nasturtium, a plant of Ranunculaceae, and is distributed in bamboo leaves, orientalis and other plants. At present, it is mainly used for the quality control of medicinal materials such as nasturtium, bamboo leaves and Chinese weed, and the quality control of traditional Chinese medicine preparations containing medicinal materials such as nasturtium, bamboo leaf and Chinese weed. The current preparation method of orientin standard substance has disadvantages such as low yield, high cost and insufficient purity. Contents of the invention [0003] The purpose of the present invention is to disclose the preparation method of orientin standard substance. [0004] The orientin standard substance of the prese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34G01N33/15
Inventor 黄泽奇周长奎张安静
Owner 黄泽奇
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