CN103588835B - A kind of method reclaiming scutellarin from waste liquid is sunk in acid - Google Patents
A kind of method reclaiming scutellarin from waste liquid is sunk in acid Download PDFInfo
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- CN103588835B CN103588835B CN201310565420.XA CN201310565420A CN103588835B CN 103588835 B CN103588835 B CN 103588835B CN 201310565420 A CN201310565420 A CN 201310565420A CN 103588835 B CN103588835 B CN 103588835B
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Abstract
The present invention discloses a kind of method reclaiming scutellarin from waste liquid is sunk in acid, belongs to effective ingredients in plant extraction and separation technology field and field of industrial waste water treatment; In waste liquid is sunk in acid, add a certain amount of pure water, leave standstill, separate out precipitation, by sedimentation and filtration, washing, adopts organic solvent recrystallization, can obtain high purity scutellarin, the present invention reclaims the scutellarin that acid is sunk in waste liquid, make use of medicinal raw material further, the method is simple to operate, and cost is low, easy suitability for industrialized production, has certain economic benefit and the value of environmental protection.
Description
Technical field
The present invention relates to a kind of method reclaiming scutellarin from waste liquid is sunk in acid, belong to effective ingredients in plant extraction and separation technology field and field of industrial waste water treatment.
Background technology
Herba Erigerontis is also known as Herba Erigerontis, for the herb of the short booth bitter fleabane of composite family bitter fleabane platymiscium, have remove obstruction in channels to relieve pain, promoting blood circulation and removing blood stasis, improve the effects such as blood microcirculation, clinically for the treatment of the diseases such as coronary heart disease, diabetes, ephrosis, apoplexy sequela, stenocardia, eighties of last century eighties, Yunnan medicine institute Zhang Renwei etc. be separated from Herba Erigerontis first Herba Erigerontis effective constituent---(have another name called scutellarin, structure is 4 ' to scutellarin, 5,6-trihydroxyflavone-7-
o-glucuronide), research and develop the preparation such as Herba Erigerontis tablet, Breviscapine on this basis, at present, the billions of unit of Herba Erigerontis series product annual value of production, Yunnan Province has been classified as focus development Chinese medicinal materials, and in Chuxiong, Lijing, the ground such as Red River carries out implant mass exploitation, processing.
" Chinese Pharmacopoeia (2010 editions) " regulation Breviscarpine is containing effective constituent---scutellarin need be greater than 90%.For a long time, from Herba Erigerontis medicinal material, the method for extraction separation and purification Breviscarpine mostly is sour heavy, then precipitation recrystallization method is obtained scutellarin; Also can adopt macroporous adsorbing resin for purification total flavones, elutriant acidifying, precipitation obtain Breviscarpine coarse-grain, then obtain highly purified scutellarin by recrystallization.Production Breviscarpine or scutellarin all have employed the heavy technique of acid, create a large amount of mother liquors, become the heavy waste liquid of acid.The pH of the heavy waste liquid of these acid is 1-2, needs just can reach emission standard with rear in a large amount of alkali, simultaneously, also remain a part of scutellarin in waste liquid, if can reclaim, herb resource can be made full use of further, BOD, TOD of reducing the heavy waste liquid of acid are equivalent, are conducive to discharge.But, have no bibliographical information on the one hand at this.
Summary of the invention
The object of the present invention is to provide a kind of method reclaiming scutellarin from waste liquid is sunk in acid, specifically comprise the steps:
(1) sinking the volume ratio of waste liquid and pure water in acid is that the ratio of 1:1 ~ 1:10 adds pure water in waste liquid is sunk in acid, leave standstill 2-12 hour, filtration is precipitated, precipitation distilled water wash 1 ~ 2 time, gained is deposited in 20 ~ 60 DEG C of vacuum-dryings 4 ~ 12 hours, obtains scutellarin coarse-grain;
(2) the scutellarin coarse-grain obtained in step (1) joins in organic solvent by the ratio being 1:5 ~ 1:20 in the volume ratio of scutellarin coarse-grain and acetone, recrystallization 1 ~ 2 time, filter, precipitate 1 ~ 2 time with identical organic solvent washing, then will be deposited in temperature is vacuum-drying 4 ~ 12 hours under the condition of 20 ~ 60 DEG C, obtains scutellarin highly finished product.
Organic solvent of the present invention is the one in acetone, ethanol or methyl alcohol.
Acid of the present invention is sunk waste liquid and is sunk waste liquid for acid that the heavy explained hereafter Breviscarpine of employing acid or scutellarin produce.
The method for detecting purity of scutellarin sample of the present invention, specifically comprises the following steps:
(1) plant and instrument: Agilent1200 palette spectrogram instrument, is furnished with quaternary pump, diode-array detector, automatic sampler, column oven, with AgilentZORBAXSB-C
18(4.6 × 250mm, 5 μm) are chromatographic column;
(2) liquid-phase condition: 0.1% phosphate aqueous solution (A)-acetonitrile (B) is moving phase, and carry out gradient elution, gradient is as follows: 0-15min, 15-40%B; Column temperature 30 ° of C, flow velocity 0.8ml/min; Determined wavelength 335nm, sample size 10 μ l;
(3) typical curve: Y=30.389c-3.8889 (r=0.9998), Y are peak area, and c is scutellarin concentration (μ g/ml);
(4) purity testing formula: scutellarin purity=scutellarin concentration/sample concentration × 100%.
Beneficial effect of the present invention is:
(1) the present invention reclaims the scutellarin that acid is sunk in waste liquid, more makes full use of herb resource;
(2) the present invention just can be recovered to highly purified scutellarin by simple method, with low cost, and easy suitability for industrialized production has good economic benefit;
(3) committed step of the present invention for add pure water in waste liquid is sunk in acid, do not pollute environment;
(4), while the present invention makes full use of herb resource, effectively can reduce the organism in the heavy waste liquid of acid, reduce TOD and BOD value, reduce waste liquid to the pollution of environment.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but scope is not limited to described content.
Embodiment 1
From waste liquid is sunk in acid, reclaim the method for scutellarin described in the present embodiment, specifically comprise the steps:
(1) sinking the volume ratio of waste liquid and pure water in acid is that the ratio of 1:5 adds pure water in waste liquid is sunk in acid, and leave standstill 2 hours, filtration is precipitated, precipitation distilled water wash 1 time, and gained is deposited in 20 DEG C of vacuum-dryings 12 hours, obtains scutellarin coarse-grain;
(2) the scutellarin coarse-grain obtained in step (1) joins in acetone by the ratio being 1:5 in the volume ratio of scutellarin coarse-grain and acetone, recrystallization 1 time, filter, 1 time is precipitated with identical washing with acetone, then being vacuum-drying 12 hours under the condition of 20 DEG C by being deposited in temperature, obtaining scutellarin highly finished product;
(3) preparation of need testing solution: get the heavy waste liquid 10ml of acid, vacuum-drying obtains solid, is configured to the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample one with methyl alcohol; Precise scutellarin coarse-grain 10mg, is mixed with methyl alcohol the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample two; Precise scutellarin highly finished product 10mg, is mixed with methyl alcohol the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample three;
(4) test the purity of sample one, two, three, measurement result is as shown in table 1.
The purity testing result of table 1. scutellarin
Embodiment 2
From waste liquid is sunk in acid, reclaim the method for scutellarin described in the present embodiment, specifically comprise the steps:
(1) sinking the volume ratio of waste liquid and pure water in acid is that the ratio of 1:10 adds pure water in waste liquid is sunk in acid, and leave standstill 12 hours, filtration is precipitated, precipitation distilled water wash 2 times, and gained is deposited in 40 DEG C of vacuum-dryings 8 hours, obtains scutellarin coarse-grain;
(2) the scutellarin coarse-grain obtained in step (1) joins in ethanol by the ratio being 1:10 in the volume ratio of scutellarin coarse-grain and ethanol, recrystallization 2 times, filter, 2 times are precipitated by identical washing with alcohol, then being vacuum-drying 9 hours under the condition of 35 DEG C by being deposited in temperature, obtaining scutellarin highly finished product;
(3) preparation of need testing solution: get the heavy waste liquid 10ml of acid, vacuum-drying obtains solid, is configured to the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample one with methyl alcohol; Precise scutellarin coarse-grain 10mg, is mixed with methyl alcohol the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample two; Precise scutellarin highly finished product 10mg, is mixed with methyl alcohol the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample three;
(4) test the purity of sample one, two, three, measurement result is as shown in table 2.
The purity testing result of table 2. scutellarin
Embodiment 3
From waste liquid is sunk in acid, reclaim the method for scutellarin described in the present embodiment, specifically comprise the steps:
(1) sinking the volume ratio of waste liquid and pure water in acid is that the ratio of 1:1 adds pure water in waste liquid is sunk in acid, and leave standstill 8 hours, filtration is precipitated, precipitation distilled water wash 2 times, and gained is deposited in 60 DEG C of vacuum-dryings 4 hours, obtains scutellarin coarse-grain;
(2) the scutellarin coarse-grain obtained in step (1) joins in methyl alcohol by the ratio being 1:8 in the volume ratio of scutellarin coarse-grain and methyl alcohol, recrystallization 2 times, filter, 2 times are precipitated by identical methanol wash, then being vacuum-drying 4 hours under the condition of 60 DEG C by being deposited in temperature, obtaining scutellarin highly finished product;
(3) preparation of need testing solution: get the heavy waste liquid 10ml of acid, vacuum-drying obtains solid, is configured to the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample one with methyl alcohol; Precise scutellarin coarse-grain 10mg, is mixed with methyl alcohol the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample two; Precise scutellarin highly finished product 10mg, is mixed with methyl alcohol the sample liquid that mass percent concentration is 100 μ g/ml, obtains sample three;
(4) test the purity of sample one, two, three, measurement result is as shown in table 3.
The purity testing result of table 3. scutellarin
Claims (1)
1. from waste liquid is sunk in acid, reclaim a method for scutellarin, it is characterized in that specifically comprising the steps:
(1) sinking the volume ratio of waste liquid and pure water in acid is that the ratio of 1:1 ~ 1:10 adds pure water in waste liquid is sunk in acid, leave standstill 2-12 hour, filtration is precipitated, precipitation distilled water wash 1 ~ 2 time, gained is deposited in 20 ~ 60 DEG C of vacuum-dryings 4 ~ 12 hours, obtains scutellarin coarse-grain;
(2) the scutellarin coarse-grain obtained in step (1) joins in organic solvent by the ratio being 1:5 ~ 1:20 in the volume ratio of scutellarin coarse-grain and organic solvent, recrystallization 1 ~ 2 time, filter, precipitate 1 ~ 2 time with identical organic solvent washing, then will be deposited in temperature is vacuum-drying 4 ~ 12 hours under the condition of 20 ~ 60 DEG C, obtains scutellarin highly finished product;
Described organic solvent is the one in acetone, ethanol or methyl alcohol.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462620A (en) * | 2003-04-22 | 2003-12-24 | 中国科学院昆明植物研究所 | Powder of flenabane and its preparation method as well as application in making drugs |
| CN101249125A (en) * | 2007-12-29 | 2008-08-27 | 重庆希尔安药业有限公司 | Herbicide composition and its preparation and application, medicament use |
| CN102188440A (en) * | 2010-03-16 | 2011-09-21 | 万生联合制药有限公司 | Preparation method of high-purity breviscapinun material used by breviscapinun injection |
| CN102614240A (en) * | 2012-04-26 | 2012-08-01 | 王祥红 | Extract containing breviscapine and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462620A (en) * | 2003-04-22 | 2003-12-24 | 中国科学院昆明植物研究所 | Powder of flenabane and its preparation method as well as application in making drugs |
| CN101249125A (en) * | 2007-12-29 | 2008-08-27 | 重庆希尔安药业有限公司 | Herbicide composition and its preparation and application, medicament use |
| CN102188440A (en) * | 2010-03-16 | 2011-09-21 | 万生联合制药有限公司 | Preparation method of high-purity breviscapinun material used by breviscapinun injection |
| CN102614240A (en) * | 2012-04-26 | 2012-08-01 | 王祥红 | Extract containing breviscapine and preparation method thereof |
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