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Method for preparing geraniin
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A novel and volumetric technology, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., to achieve the effects of large-scale production operations, less pollution, and less energy consumption
Inactive Publication Date: 2011-04-13
SUZHOU PAITENG BIOLOGICAL MEDICAL TECH
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[0006] In the prior art, there is no report on the preparation process applicable to the industrialized large-scale production of high-purity geranolin
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Embodiment 1
[0025] Take 10Kg of fresh geranium stems and leaves, add 80L water to soak for 18 hours, squeeze and filter, take the filtrate, absorb it through an activated carbon column, elute with 75% ethanol, collect 3 times the column volume eluate, recover ethanol under reduced pressure and concentrate , adsorbed by D101 macroporous adsorption resin column, eluted with 50% ethanol, collected 3 times the column volume eluate, recovered ethanol under reduced pressure and concentrated, added methanol for crystallization, separated crystallization, washed and dried to obtain yellow crystal-牻 Geranin 78.4g, detected by HPLC, the purity is 96.2%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.
Embodiment 2
[0027] Take 10Kg of fresh geranium stems and leaves, add 120L water to soak for 36 hours, squeeze and filter, take the filtrate, absorb it through an activated carbon column, elute with 85% ethanol, collect 8 times the column volume eluate, recover ethanol under reduced pressure and concentrate , adsorbed by H50 macroporous adsorption resin column, eluted with 70% ethanol, collected 8 times the column volume eluate, recovered ethanol under reduced pressure and concentrated, added methanol for crystallization, separated crystallization, washed and dried to obtain yellow crystal-牻 Geranin 82.7g, detected by HPLC, the purity is 95.0%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.
Embodiment 3
[0029] Take 10Kg of fresh geranium stems and leaves, add 100L water to soak for 24 hours, squeeze and filter, take the filtrate, absorb it through an activated carbon column, elute with 80% ethanol, collect 5 times the column volume eluate, recover ethanol under reduced pressure and concentrate , adsorbed by AB8 macroporous adsorption resin column, eluted with 60% ethanol, collected 5 times the column volume eluate, recovered ethanol under reduced pressure and concentrated, added methanol for crystallization, separated crystallization, washed and dried to obtain yellow crystal-牻 Geranin 78.4g, detected by HPLC, the purity is 96.2%, UV, IR, MS, 2 HNMR, 13 The data characterizing its physical properties such as CNMR are consistent with the prior art.
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Abstract
The invention relates to a method for preparing geraniin, which is simple and convenient to operate and has low pollution and low energy consumption. The method comprises the following steps of: soaking fresh geranium stem leaves into water for 18 to 36 hours, squeezing and filtering, taking filtrate, adsorbing the filtrate through an active carbon column, eluting the active carbon column by using 75 to 85 percent ethanol, collecting eluant, reclaiming the ethanol under reduced pressure and concentrating, adsorbing the concentrate through a macroporous adsorptive resin column, eluting the macroporous adsorptive resin column by using ethanol, collecting eluant, reclaiming the ethanol under reduced pressure and concentrating, adding methanol for crystallization, and separating, washing and drying the crystal to obtain the geraniin. The method for preparing the geraniin has high product purity and is easy to realize industrialized amplification.
Description
technical field [0001] The invention relates to a preparation method of geraniol, in particular to a preparation method of extracting geraniol from plants. Background technique [0002] Geraniin, molecular formula: C 41 h 28 o 27 , molecular weight: 952.656, CAS accession number: 60976-49-0. It is present in various plants of Aceraceae, Echinaceae, Nymphaceae, and Nymphaeaceae. Among them, Geranium wilfordi Maxim., a plant of the family Aceraceae, has a higher content and its sources are abundant. Its molecular formula is as follows: [0003] [0004] The dry aerial part of Geranium wilfordii Maxim., a plant of the family Borealaceae, is used as a traditional Chinese medicine, Geranium wilfordii Maxim. [0005] Modern studies have shown that geraniol has various activities such as anti-oxidation, anti-inflammation, anti-virus, anti-HIV, and liver protection, and it is also used as a raw material for the synthesis of other active derivatives. [0006] In the prior ar...
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