CN101735191A - Method for preparing flavonoid component capable of stopping nitrosation reaction - Google Patents
Method for preparing flavonoid component capable of stopping nitrosation reaction Download PDFInfo
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- CN101735191A CN101735191A CN200810231013A CN200810231013A CN101735191A CN 101735191 A CN101735191 A CN 101735191A CN 200810231013 A CN200810231013 A CN 200810231013A CN 200810231013 A CN200810231013 A CN 200810231013A CN 101735191 A CN101735191 A CN 101735191A
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- hawthorn
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- methanol
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Abstract
The invention discloses a method for preparing flavonoid component capable of stopping nitrosation reaction, comprising the following steps: grinding hawthorns, soaking the ground hawthorn in 60-100 percent ethanol of 20-30 DEG C to extract hawthorn flavonoid component, recovering the ethanol, proportioning with ethyl acetate/water, separating the obtained extract with the silica gel column chromatography, carrying out gradient elution with chloroform-methanol and collecting the part eluted by the chloroform-methanol at the ratio of 9:1-8:2. Due to the adoption of the technical scheme, about 30 g of the hawthorn flavonoid component can be extracted from every 1 kg of hawthorns. Because the hawthorn trees are distributed very extensively in China, the raw material of hawthorn can be very easy to obtain, and the production cost can be effectively reduced. Sufficient raw materials are provided for the development of the health-care cigarette, and a new way for deep processing the hawthorn is provided for the hawthorn grower.
Description
Technical field
The invention belongs to the preparation of natural organic-compound, relate to a kind of preparation method of flavonoid component of energy stopping nitrosation reaction
Background technology
2003, clear and definite Chinese tobacco is the industry development direction with " Chinese style cigarette " in " Chinese tobacco development in science and technology outline " that State Tobacco Monopoly Bureau formulates, the world trends of cigarette harm reduction are complied with in proposition, realize the low evilization of product, fully excavate Chinese traditional Chinese herbal medicine resource, the utilization modern high tech method is made " Chinese style cigarette " core technology.A large amount of modern pharmacology experiments show that the herbal medicine functional ingredient is the scavenging agent of oxyradical and the blocker of lipid peroxidation; can prevent the oxidation toxic action of radical pair cell composition effectively; protection cytolemma phosphorus and protein are not subjected to the damage of smoking; can obviously suppress carcinogenic substances such as carbon monoxide in the cigarette smoke, benzopyrene [α], nitrosamine; remove unnecessary free radical; repair the soft tissue that smoking causes human respiratory tract's oxidation; make it to reach reduction and equilibrium state, have multiple efficacies such as the lung tissue of avoiding damage, heart trouble and other disease generation.Current, smoking and health problem have become the problem that the whole world is paid close attention to, and fall the existing a lot of successful examples of harmful purpose by Chinese herbal medicine extract being added to reach in the tobacco.Because forming the precursor of tobacco-specific nitrosamine mainly is nicotiana alkaloids, in the nicotiana alkaloids,, secondly be nornicotine based on nicotine, also have anatabine and neonicotine etc., therefore reduce nitrosamine total content in the tobacco and can block the nitrosation reaction of nicotine and achieve the goal.The basic substance that herbal medicine applies to tobacco harm reduction, control evil is the active chemical that wherein contains, remove free radical, the antioxygenation except having such as the flavonoid compound that is rich in the herbal medicine, all right stopping nitrosation reaction, thereby tobacco-specific nitrosamine total content in the reduction main flume has good application prospects in the exploitation of health promoting cigarette.And prepare a large amount of, flavones is the key factor of this industry development cheaply.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of flavonoid component of energy stopping nitrosation reaction, raw material is easy to get, and is with low cost.
For achieving the above object, the present invention adopts following technical scheme: a kind of preparation method of flavonoid component of energy stopping nitrosation reaction, be that hawthorn is pulverized, ethanol with 60-100% soaks extraction down at 20～30 ℃, reclaim behind the ethanol with ethyl acetate/water dispenser, the medicinal extract that obtains is separated through silica gel column chromatography,, collect chloroform-methanol 9: 1-8: 2 wash-out parts with the chloroform-methanol gradient elution.
With the hawthorn crushed after being dried, extract with 95% ethanol soaking at room temperature, with ethyl acetate/water dispenser, the medicinal extract that obtains is separated through silica gel column chromatography behind the recovery ethanol, with the chloroform-methanol gradient elution, collect chloroform-methanol 9: 1-8: 2 wash-out parts.
After adopting technique scheme, can extract from per 1 kilogram of hawthorn about Fructus Crataegi total flavones component 30 grams, because hawthorn is very extensive in the distribution of China, it is very easy therefore to obtain raw material, and can effectively reduce production costs.This both provided competent raw material for the exploitation of health promoting cigarette, had also found a new outlet for orchard worker's product deep processing.
Embodiment
Embodiment 1: with 200g hawthorn crushed after being dried, the ethanol soaking at room temperature with 95% is extracted, and with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 10 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 6 grams.
Embodiment 2: with 500g hawthorn crushed after being dried, the ethanol soaking at room temperature with 95% is extracted, and with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 30 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 15 grams.
Embodiment 3: with 1000g hawthorn crushed after being dried, the ethanol with 95% soaks extraction under 30 ℃ of temperature, with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 50 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 25 grams.
Embodiment 4: with 400g hawthorn crushed after being dried, the ethanol soaking at room temperature with 60% is extracted, and with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 22 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 11 grams.
Embodiment 5: with 700g hawthorn crushed after being dried, the ethanol with 99% soaks extraction under 20 ℃ of temperature, with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 36 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 22 grams.
Embodiment 6: with 600g hawthorn crushed after being dried, the ethanol with 70% soaks extraction under 25 ℃ of temperature, with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 29 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 17 grams.
Embodiment 7: with 800g hawthorn crushed after being dried, the ethanol with 90% soaks extraction under 28 ℃ of temperature, with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 41 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 25 grams.
Embodiment 8: the 300g hawthorn is pulverized, and the ethanol with 80% soaks extraction under 22 ℃ of temperature, with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 22 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 10 grams.
Embodiment 9: the 900g hawthorn is pulverized, and the ethanol with 85% soaks extraction under 25 ℃ of temperature, with ethyl acetate/water dispenser, obtains ethyl acetate medicinal extract 45 grams behind the decompression recycling ethanol.Ethyl acetate medicinal extract is separated through silica gel column chromatography, with the chloroform-methanol gradient elution.Collect chloroform-methanol 9: 1-8: 2 wash-outs partly obtain Fructus Crataegi total flavones component 26 grams.
Give to take in advance the rat of certain proportion nicotine and Sodium Nitrite with gained Fructus Crataegi total flavones component in the gastric infusion mode, collect rat twenty-four-hour urine liquid and measure the content of urine Central Asia nitration product N-nitrosonornicotine with GC-TEA.By with blank comparison rat urine in N-nitrosonornicotine content descended 15%～30%, show that the flavonoid component in the hawthorn can pass through stopping nitrosation reaction, reach the purpose that reduces tobacco-specific nitrosamine total content in the main flume.
Claims (2)
1. the preparation method of the flavonoid component of an energy stopping nitrosation reaction, it is characterized in that: hawthorn is pulverized, ethanol with 60-100% soaks extraction down at 20～30 ℃, reclaim behind the ethanol with ethyl acetate/water dispenser, the medicinal extract that obtains is separated through silica gel column chromatography, with the chloroform-methanol gradient elution, collect chloroform-methanol 9: 1-8: 2 wash-out parts.
2. the preparation method of the flavonoid component of energy stopping nitrosation reaction as claimed in claim 1, it is characterized in that: with the hawthorn crushed after being dried, extract with 95% ethanol soaking at room temperature, reclaim behind the ethanol with ethyl acetate/water dispenser, the medicinal extract that obtains is separated through silica gel column chromatography, with the chloroform-methanol gradient elution, collect chloroform-methanol 9: 1-8: 2 wash-out parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200810231013A CN101735191A (en) | 2008-11-24 | 2008-11-24 | Method for preparing flavonoid component capable of stopping nitrosation reaction |
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| CN200810231013A CN101735191A (en) | 2008-11-24 | 2008-11-24 | Method for preparing flavonoid component capable of stopping nitrosation reaction |
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| CN101735191A true CN101735191A (en) | 2010-06-16 |
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| CN200810231013A Pending CN101735191A (en) | 2008-11-24 | 2008-11-24 | Method for preparing flavonoid component capable of stopping nitrosation reaction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110432537A (en) * | 2012-10-09 | 2019-11-12 | R.J.雷诺兹烟草公司 | The flavonoid composition of the methylation of O- derived from tobacco |
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2008
- 2008-11-24 CN CN200810231013A patent/CN101735191A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110432537A (en) * | 2012-10-09 | 2019-11-12 | R.J.雷诺兹烟草公司 | The flavonoid composition of the methylation of O- derived from tobacco |
| US11412775B2 (en) | 2012-10-09 | 2022-08-16 | R.J. Reynolds Tobacco Company | Tobacco-derived composition |
| CN110432537B (en) * | 2012-10-09 | 2022-08-19 | R.J.雷诺兹烟草公司 | Tobacco-derived O-methylated flavonoid compositions |
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