CN102133487A - Infrared extraction and reaction device and use thereof - Google Patents

Infrared extraction and reaction device and use thereof Download PDF

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Publication number
CN102133487A
CN102133487A CN2010101001677A CN201010100167A CN102133487A CN 102133487 A CN102133487 A CN 102133487A CN 2010101001677 A CN2010101001677 A CN 2010101001677A CN 201010100167 A CN201010100167 A CN 201010100167A CN 102133487 A CN102133487 A CN 102133487A
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infrared
extraction
infrared light
light supply
reaction unit
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CN2010101001677A
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Chinese (zh)
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段更利
李嫣
陈益乐
段昊天
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Fudan University
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Fudan University
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Abstract

The invention belongs to the field of chemical analysis and in particular relates to an infrared extraction and reaction device and use thereof. The infrared extraction and reaction device consists of an infrared light source capable of generating infrared radiation, an adjustable rheostat, a lamp shade, a condensing tube and a bracket, wherein the adjustable rheostat controls the power of the infrared light source; the infrared light source is positioned at a certain position below an extraction or reaction container; and a container opening is connected with the condensing tube to make a solvent reflow in the process of the infrared radiation. The device can realize fast extraction of active ingredients in traditional Chinese medicines and fruits and vegetables and fast synthesis of organic compounds through the infrared radiation emitted from the infrared light source. The device is simple in design, efficient in heat transfer, and economical and environmentally-friendly.

Description

A kind of infrared extraction and reaction unit and uses thereof
Technical field
The invention belongs to chemical analysis field, be specifically related to a kind of infrared extraction and reaction unit and uses thereof.
Background technology
Ultrared wave-length coverage is 0.75 μ m-1000 μ m, between electromagnetic wave and visible light, outwards propagates with the form of radiation.Prior art discloses the heatable substance ambient air not because infra-red radiation directly acts on material, thus be different from other as convection current and conduct the heat propagation mode, infra-red radiation is more efficient than other thermaltransmission modes.Studies show that when the absorbing wavelength of the wavelength in infra-red radiation source and heating object was consistent, this material was easy to absorb infrared energy.Material molecule can make the energy of photon be transformed into the vibration or the rotational energy of molecule fully after absorbing infrared energy.At present, commercially available infrared light supply can send the continuous spectrum of certain intensity and mainly concentrate on 1.72-16.66 μ m place that (its pairing wave-number range just in time is 600-5800cm -1).And the infrared vibration absworption peak of most of molecule all drops in this scope.Studies show that, when infra-red radiation was applied to the Chinese medicine extracts active ingredients, infra-red radiation entered in the material body, can strengthen the motion of its component molecule, by force do the time spent to the constraint that is enough to break away from heating object when the component molecular motion, then this component is extracted out.Studies show that in addition when infrared radiation was applied to organic synthesis, the energy that infra-red radiation passes out was caused the molecular vibrational energy order transition by molecule absorption, the contact between the accelerated reaction thing molecule reaches the purpose of synthetic reaction.Similar to microwave, infra-red radiation propagates into the heating object surface with the speed of light, and has partial radiation to penetrate interior of articles just to be absorbed, and having to conduct heat fast and object surfaces externally and internally characteristics such as have a narrow range of temperature.
Extracts active ingredients and organic synthesis in traditional Chinese medicine and the fruits and vegetables, normally reflux by water-bath, reach and extract or the synthetic reaction purpose thereby promptly conduct heat by WATER AS FLOW MEDIUM, Shang Weijian adopts infrared abstraction reaction device to carry out the report of extracts active ingredients in Chinese medicine and the fruits and vegetables or synthetic reaction.So this area researcher begins to pay close attention to the relevant infrared more efficiently abstraction reaction device that conducts heat of development, for modern Microwave Extraction reaction technology, infrared abstraction reaction device need not special instrument and equipment, compares more easy economy.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of heat transfer infrared more efficiently abstraction reaction device, infrared abstraction reaction device of the present invention can be applied to extracts active ingredients and organic synthesis in Chinese medicine and the fruits and vegetables.
Infrared abstraction reaction device of the present invention is characterized in that, its infrared light supply (1), and adjustable rheostat (2), condenser pipe (3) support (4), reaction vessel (6) is formed, and lampshade (5) covers on the infrared light supply top.
Among the present invention, infrared light supply (1) is a radiation source, produces infra-red radiation;
Among the present invention, radiation source mainly concentrates on infrared ray bulb between the 0.6 μ m-20 μ m, infrared lamp, infrared incandescent lamp etc. for producing wave-length coverage, and other can produce the infrared light supply of wave-length coverage in infrared wavelength range,
Described infrared light supply is positioned at and extracts or a distance, reaction vessel (6) below, and preferred infrared light supply is positioned at and extracts or 1-20cm place, reaction vessel below, and it makes container accept evenly infra-red radiation fully.
Among the present invention, the power of adjustable rheostat (2) control infrared light supply.
Among the present invention, the vessel port of reaction vessel (6) and condenser pipe (3) join, and make solvent obtain refluxing in the infrared radiation process.
Apparatus of the present invention design is easy, and cost is low, economical and efficient,
Apparatus of the present invention can be applicable to the extraction and the organic synthesis of active ingredient in Chinese medicine and the fruits and vegetables.
Another purpose of the present invention provides the method for utilizing above-mentioned infrared radiation device to extract active ingredient in the Chinese medicine, and this method may further comprise the steps:
With the Chinese medicine grinding and sieving, get an amount of Chinese drugs powder then in the 50mL round-bottomed flask, add a certain amount of extractant, open infrared light supply and shine, timing when treating that the condenser pipe lower end begins solvent refluxing to occur, extract certain hour after, close infrared light supply, treat that round-bottomed flask cooling back benefit is heavy, select suitable chromatogram analysis method to analyze behind the centrifuging and taking supernatant liquid filtering, obtain measurement result.
Another purpose of the present invention provides the method for utilizing above-mentioned infrared radiation device organic synthesis simple compounds, and this method may further comprise the steps:
Get reactant in right amount in round-bottomed flask, add a certain amount of catalyst according to actual conditions, opening infrared light supply shines, timing when treating that the condenser pipe lower end begins solvent refluxing to occur, behind the reaction certain hour, close infrared light supply, question response bottle cooling back is the processing reaction product further, calculated yield.
For the ease of understanding, below will describe in detail of the present invention by concrete drawings and Examples.It needs to be noted, instantiation and accompanying drawing only are in order to illustrate, obviously those of ordinary skill in the art can illustrate according to this paper, within the scope of the invention the present invention is made various corrections and change, and these corrections and change are also included in the scope of the present invention.
Description of drawings
Fig. 1 is the structural representation of the infrared abstraction reaction device of the present invention,
Wherein, the 1st, infrared light supply, the 2nd, adjustable rheostat,, the 3rd, condenser pipe, the 4th, support, the 5th, lampshade, the 6th, reaction vessel.
The specific embodiment
The structure of embodiment 1 infrared abstraction reaction device
The structure of exemplary infrared abstraction reaction device as shown in Figure 1, it comprises infrared light supply (1), adjustable rheostat (2), condenser pipe (3) support (4), reaction vessel (6) is formed, and lampshade (5) covers on the infrared light supply top, infrared light supply (1) is a radiation source, produces infra-red radiation; Described radiation source mainly concentrates on infrared ray bulb between the 0.6 μ m-20 μ m, infrared lamp, infrared incandescent lamp etc. for producing wave-length coverage, and other can produce the infrared light supply of wave-length coverage in infrared wavelength range, described infrared light supply is positioned at and extracts or 1-20cm place, reaction vessel (6) below, and it makes container accept evenly infra-red radiation fully; The power of described adjustable rheostat (2) control infrared light supply; The vessel port of described reaction vessel (6) and condenser pipe (3) join, and make solvent obtain refluxing in the infrared radiation process.
8 kinds of content of effective in the embodiment 2 infra-red radiation assisted extraction high-efficient liquid phase chromatogram technique analysis reds sage root
Instrument and material:
Instrument: Tianjin, island CL-10 type liquid chromatograph (comprising SPD-10A UV-detector and CTO-10A column oven, 20 μ L hand sampling systems, chromatographic work station), An Disheng board hard infra-red radiation, Millipore Direct-Q pure water generator.
Material: the red sage root (Shandong, the place of production, lot number: 091117,090923; Henan, the place of production, lot number: 090314; Jiangsu, the place of production, lot number: 081207).Acetonitrile (the U.S. world, chromatographically pure), methyl alcohol (Jiangsu Chinese nation, chromatographically pure), formic acid (analyzing pure), the deionization pure water is made by the MilliporeDirect-Q pure water generator, and danshensu, protocatechuic acid, protocatechualdehyde, tanshin polyphenolic acid B, dihydrotanshinone, Cryptotanshinone, Tanshinone I and tanshinone IIA standard items derive from Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
40 mesh sieves are crossed in the red rooted salvia pulverizing back in the different places of production, respectively get the 0.1g Danshen Root then in the 50mL round-bottomed flask, add the 15mL70% methanol aqueous solution, infra-red radiation extracted after 15 minutes, and sample introduction behind the centrifuging and taking supernatant liquid filtering of the heavy back of benefit obtains measurement result.
Embodiment 3 infra-red radiations are assisted the salicylate methyl esters
Instrument and material:
Instrument: Tianjin, island CL-10 type liquid chromatograph (comprising SPD-10A UV-detector and CTO-10A column oven, 20 μ L hand sampling systems, chromatographic work station), An Disheng board hard infra-red radiation, Millipore Direct-Q pure water generator.
Material: salicylic acid (traditional Chinese medicines reagent group analyzes pure), methyl alcohol (Jiangsu Chinese nation, chromatographically pure), the concentrated sulfuric acid (traditional Chinese medicines reagent is analyzed pure), the gaultherolin reference substance derives from Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Take by weighing salicylic acid 3g and place the 50mL round-bottomed flask, add 10mL methyl alcohol, heating makes dissolving, slowly adds concentrated sulfuric acid 2mL then, and jolting evenly back adds zeolite, places the infrared light supply top.Open condenser pipe and infrared light supply, stop infra-red radiation behind the irradiation 2h.Put the unnecessary methyl alcohol of cold back water bath method, use saturated NaHCO then 3Regulator solution pH pours out liquid in the round-bottomed flask to separatory funnel to slightly acid, leaves standstill to treat to collect lower floor's liquid after its layering.Undertaken quantitatively by the HPLC method after diluting certain multiple then, and calculate productive rate.

Claims (7)

1. infrared extraction and reaction unit is characterized in that it is by infrared light supply (1), adjustable rheostat (2), condenser pipe (3) support (4), reaction vessel (6) is formed, lampshade (5) covers on the infrared light supply top, and infrared light supply is positioned at and extracts or reaction vessel (6) below 1-20cm distance.
2. by described infrared extraction of claim 1 and reaction unit, it is characterized in that described infrared light supply (1) is a radiation source, produce infra-red radiation.
3. by described infrared extraction of claim 2 and reaction unit, it is characterized in that, described radiation source for can produce wave-length coverage between 0.6 μ m-20 μ m infrared ray bulb, infrared lamp or infrared incandescent lamp or other can produce the infrared light supply of wave-length coverage in infrared wavelength range.
4. by described infrared extraction of claim 1 and reaction unit, it is characterized in that the power of described adjustable rheostat (2) control infrared light supply.
5. by described infrared extraction of claim 1 and reaction unit, it is characterized in that the vessel port of reaction vessel (6) and condenser pipe (3) join, make solvent in the infrared radiation process, obtain refluxing.
6. described infrared extraction of claim 1 and the reaction unit purposes in the active ingredient in extracting Chinese medicine or fruits and vegetables.
7. described infrared extraction of claim 1 and the purposes of reaction unit in organic synthesis.
CN2010101001677A 2010-01-22 2010-01-22 Infrared extraction and reaction device and use thereof Pending CN102133487A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103512981A (en) * 2012-06-19 2014-01-15 复旦大学 Method for ion liquid-infrared assisted extraction of effective components of traditional Chinese medicine
CN105661241A (en) * 2016-03-23 2016-06-15 抚松县飓峰参业有限公司 Beverage containing radix ginseng rubra liquid and production method of beverage
CN107376417A (en) * 2017-09-07 2017-11-24 合肥海正环境监测有限责任公司 A kind of movable steady flat extracts device admittedly
CN107774006A (en) * 2016-08-26 2018-03-09 段昊天 The infrared assisted extraction and reaction system of a kind of controllable temperature
CN109320486A (en) * 2017-08-01 2019-02-12 复旦大学 A kind of method of amentoflavone in infrared extraction Selaginella tamariscina
CN111558233A (en) * 2020-05-22 2020-08-21 青海省药品检验检测院 Splash-proof device that backward flow was drawed

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2334403Y (en) * 1997-01-16 1999-08-25 甘肃省医疗机械厂 Overflow-proof porous far infrared radiation heating traditional Chinese medicine decocting machine
CN200945379Y (en) * 2006-06-08 2007-09-12 复旦大学 Microwave aiding- single point microwave extracting device
CN101816842A (en) * 2010-01-20 2010-09-01 复旦大学 Far infrared radiation auxiliary extracting system

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2334403Y (en) * 1997-01-16 1999-08-25 甘肃省医疗机械厂 Overflow-proof porous far infrared radiation heating traditional Chinese medicine decocting machine
CN200945379Y (en) * 2006-06-08 2007-09-12 复旦大学 Microwave aiding- single point microwave extracting device
CN101816842A (en) * 2010-01-20 2010-09-01 复旦大学 Far infrared radiation auxiliary extracting system

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103512981A (en) * 2012-06-19 2014-01-15 复旦大学 Method for ion liquid-infrared assisted extraction of effective components of traditional Chinese medicine
CN105661241A (en) * 2016-03-23 2016-06-15 抚松县飓峰参业有限公司 Beverage containing radix ginseng rubra liquid and production method of beverage
CN107774006A (en) * 2016-08-26 2018-03-09 段昊天 The infrared assisted extraction and reaction system of a kind of controllable temperature
CN109320486A (en) * 2017-08-01 2019-02-12 复旦大学 A kind of method of amentoflavone in infrared extraction Selaginella tamariscina
CN107376417A (en) * 2017-09-07 2017-11-24 合肥海正环境监测有限责任公司 A kind of movable steady flat extracts device admittedly
CN111558233A (en) * 2020-05-22 2020-08-21 青海省药品检验检测院 Splash-proof device that backward flow was drawed

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Application publication date: 20110727