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Xanthoceraside preparation method

A technology of sorbiflorin and sorbifolin, applied in the field of medicine

Active Publication Date: 2014-01-01
SHENYANG PHARMA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods have many steps, so the loss of the compound in the preparation process is too large, causing the final yield to be too low; in addition, because the operation of macroporous adsorption resin enrichment or solvent extraction is often used, not only the macroporous adsorption resin itself is due to the synthetic Residues are easy to be generated during the process and the samples are polluted, and the amount of organic solvents is large, the cost is high, flammable and explosive, which is not conducive to environmental protection, and the damage to the body of workers is relatively large, and the safety is poor; in addition, high-speed countercurrent chromatography The cost of equipment such as methods is relatively high, which is not conducive to the development of large-scale production of enterprises

Method used

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  • Xanthoceraside preparation method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 100 g of Xantho sorbifolia husks crushed into 20 meshes, use 10 times the volume of 50% ethanol at a volume percentage concentration of 65°C, heat and reflux for 3 times for 3 hours / time, recover the solvent, and concentrate to obtain a crude extract , the crude extract is separated and purified by normal-phase silica gel column chromatography with a mesh number of 100-200, and is eluted with chloroform-methanol or dichloromethane-methanol with a volume ratio of 7:1 and 2:1 respectively , heating to reflux, recovering the solvent under reduced pressure, enriching to obtain the xanthoside fraction, placing it at room temperature, using methanol-water solvent system for recrystallization, and obtaining refined high-purity xanthoside after repeated recrystallization; the purity is 99.5%, the yield is 0.047% 0 .

[0032] According to the method of the previous patent (publication number: CN1626545, authorized announcement number: CN1281616C), 100 g of Xantho sorbifoli...

Embodiment 2

[0034] Take 150 g of radix sorbifolia husks crushed into 30 meshes, use 8 times the volume of 70% ethanol, temperature 70°C, heat and reflux for extraction, time 2 hours / time, extract twice, heat and reflux, and recover the solvent under reduced pressure , the extract obtained after concentration is separated and purified by normal-phase silica gel column chromatography with a mesh number of 200-300, and chloroform-methanol or dichloromethane-methanol with a volume ratio of 8:1 and 3:1 is used as the eluting solvent Elution, recovery of the solvent under reduced pressure, enrichment to obtain the fraction of xanthosides, and crude saponins; recrystallization with methanol, repeated recrystallization to obtain refined high-purity xanthosides; the purity is 98.9%, The yield is 0.048% 0 .

[0035] According to the method of the previous patent (publication number: CN1626545, authorization announcement number: CN1281616C), 150 g of Xantho sorbifolia husks were also crushed into 3...

Embodiment 3

[0037] Take 150 g of radix sorbifolia husks crushed into 30 meshes, use 8 times the volume of 65% ethanol, temperature 70°C, heat and reflux extraction, time 2.5 hours / time, extract 3 times, heat and reflux, and reduce pressure to recover the solvent , the extract obtained after concentration is separated and purified by normal-phase silica gel column chromatography with a mesh number of 200-300, and chloroform-methanol or methylene chloride-methanol with a volume ratio of 7:1 and 3:1 is used as the eluting solvent Elution, recovery of the solvent under reduced pressure, enrichment to obtain the fraction of xanthosides, and crude saponins; recrystallization with methanol, repeated recrystallization to obtain refined high-purity xanthosides; the purity is 98.9%, The yield is 0.051% 0 .

[0038] According to the method of the previous patent (publication number: CN1626545, authorization announcement number: CN1281616C), 150 g of Xantho sorbifolia husks were also crushed into 30...

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Abstract

The invention belongs to the field of medical technology and relates to a new method for preparing xanthoceraside in shinyleaf yellowhorns. The highly purified xanthoceraside can be prepared efficiently with the preparation method. The preparation method is easy and convenient to use and reliable and reduces redundant intermediate operation steps, thus, product loss is reduced, and the yield of the preparation method is obviously increased compared with that of a former method. Crude extract is directly processed with a silica gel column, eluted with the chloroform / dichloromethane-methyl alcohol eluent with the volume ratio of 10:1-7:1, the ethyl acetate-methyl alcohol eluent with the volume ratio of 10:1-5:1 or the acetone-methyl alcohol eluent with the volume ratio of 10:1-6:1, and then eluted with the chloroform / dichloromethane-methyl alcohol eluent with the volume ratio of 6:1-2:1, the ethyl acetate-methyl alcohol eluent with the volume ratio of 4:1-1:1 or the acetone-methyl alcohol eluent with the volume ratio of 5:1-3:1, solvent recovery, purification and recrystallization are performed, and finally the xanthoceraside is obtained.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a new method for preparing sorbiflora radicis glucoside. Background technique [0002] Xanthocerassorbifolia Bunge belongs to Sapindaceae ( Sapindaceae ) Xanthocarpus plants, one genus and one species, shrubs or trees, distributed in Liaoning, Hebei, Shaanxi and other provinces in my country. Its heartwood, stems and fruits can be used as medicine. It has the effects of expelling wind and dampness, reducing swelling and relieving pain, and astringing dry yellow water. It was once listed in the 2005 edition of "The Pharmacopoeia of the People's Republic of China". [0003] Studies in recent years have shown that sorbiflora glucoside (also known as sorbiflora saponin E in literature reports) is the main active ingredient of radix sorbifolium, which has anti-inflammatory, anti-tumor, inhibiting HIV protease, improving learning and memory, and improving human anti-diabetes, etc. ef...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00
Inventor 孟大利宁科权宋智林张辘辘
Owner SHENYANG PHARMA UNIVERSITY
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