CN201168460Y - Liquor-liquor-liquor three-phase extraction plant - Google Patents
Liquor-liquor-liquor three-phase extraction plant Download PDFInfo
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- CN201168460Y CN201168460Y CNU2007200882411U CN200720088241U CN201168460Y CN 201168460 Y CN201168460 Y CN 201168460Y CN U2007200882411 U CNU2007200882411 U CN U2007200882411U CN 200720088241 U CN200720088241 U CN 200720088241U CN 201168460 Y CN201168460 Y CN 201168460Y
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Abstract
The utility model provides a liquid-liquid-liquid three-phase micro-extracting device, which at least comprises a sample bottle and a bottle cork, wherein, the bottle cork is positioned on a bottle mouth of the sample bottle; a small hole is arranged in the bottle cork; an inside inserting pipe is filled in the small hole; the upper part of the inside inserting pipe is connected with the sample bottle through the small hole. The inside diameter of the upper part of the inside inserting pipe is larger than the inside diameter of the lower part. The sample bottle is a common penicillin reagent bottle or other glass bottle, and a magneton is contained in the sample bottle. A micro-injector needlepoint and an expensive hollow fibrous membrane are substituted by the cheap inside inserting pipe, the volume of extracting agents stored by the inside inserting pipe is large; the extracting amount is larger than the extracting amount from the traditional liquid-liquid-liquid three-phase micro-extraction; the extracting efficiency is high; the consumption of organic solvents is small; therefore, the analysis cost is greatly reduced. The liquid-liquid-liquid three-phase micro-extracting device has the advantages of simple operating method, easy operation and high extracting efficiency, and is very suitable for the extraction and the enrichment of complex biological and environmental samples.
Description
Technical field
The utility model relates to a kind of liquid-phase micro-extraction device, particularly a kind of liquid-liquid-liquid three phase extraction apparatus.
Background technology
The sample pre-treatments technology has material impact to analysis result, receives much attention always.The preconditioning technique of extensive use at present has liquid-liquid extraction (LLE), SPE (SPE), SPME (SPME), membrane extraction etc.Classical liquid liquid extraction plant is complex operation in the use, is difficult for realizing automation.Solid phase extraction techniques is rapidly developed in a lot of fields with advantage such as efficient, reliable, that solvent load is few, but it needs wash-out, and purifying substance is to satisfy the requirement of Instrumental Analysis such as GC or HPLC.SPME is a kind of solvent-free sample pre-treatments technology, the centralized procurement sample, extract, concentrate in one, have advantages such as simple, fast and easy, extensive use on environmental sample, food and medicine, but solid phase micro-extraction extraction head is more expensive, service life is short, repeatedly uses also there is cross-contamination issue special desorption apparatus of need also during with the HPLC coupling with it.Liquid-phase micro-extraction is quick, accurate, highly sensitive, the eco-friendly novel pretreatment technology that grows up along with the development of environmental analysis in modern age technology, it combines the advantage of liquid-liquid extraction and SPME, required organic solvent is few, simple to operate, treasury is got, purifying, concentrate in one the step finish, highly sensitive, concentration effect is good.This technology not only can be used separately, also can with gas-chromatography, liquid chromatogram, Capillary Electrophoresis, gas chromatography-mass spectrum, liquid chromatograph mass spectrography.Liquid-phase micro-extraction has the liquid-phase micro-extraction technology of two-phase and the liquid-phase micro-extraction of three-phase (liquid-liquid-liquid micro-extraction) technology.Liquid-liquid-liquid micro-extraction technique (LLLME) because of its stronger antijamming capability, can effectively be removed the interference of complicated ingredient in the sample substrate as a kind of novel sample-pretreating method, can be used for complicated biology, the processing of environmental sample.The thickness of liquid film of early stage liquid-liquid-liquid micro-extraction device is controlled easily, because liquid film all is new during each the extraction, so there is not memory effect, but, and the amount of organic solvent more (50-150 μ l) along with thereby the prolongation liquid film of time of extraction and instability that the drop on the needle point can become cause the reappearance of testing bad.At present common have film liquid-phase micro-extraction device and a doughnut liquid-phase micro-extraction device.Their acceptance adopts film or doughnut to protect mutually, and stability is better relatively, thereby mixing speed can improve slightly, yet still has some problems in experiment:
For film liquid-phase micro-extraction device: its acceptance relies on the surface tension between liquid and solid to be suspended on the needle point mutually purely, makes that the extractant volume can not be too big, and suitably increases the sensitivity that the extractant volume helps improving extraction efficiency and method; The character and the problem of accepting to be complementary mutually, the problem of service life and cross pollution that also have liquid film simultaneously.
For doughnut liquid-phase micro-extraction device, have the following disadvantages:
(1) doughnut costs an arm and a leg.
(2) polarity between organic facies and the doughnut need be mated, and could organic facies be fixed in the microvoid of doughnut effectively.
(3) be fixed on organic solvent on the micropore except polarity will be complementary with doughnut, also must satisfy water-soluble less, non-volatile, low viscosity and high Korg/d value.If want high Korg/d value just to select water-soluble big organic solvent for use inevitably, will sacrifice the stability and the service life of liquid film like this.The kind of alternative like this organic solvent is less.
(4) after the doughnut extraction, extraction phase is difficult to take out.
(5) there is cross pollution in the doughnut extraction.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the utility model provides a kind of liquid-phase micro-extraction device, and this device is simple, easy to operate, reappearance is better, sensitivity is higher, and can realize auto injection.
Realize that the technical scheme that the utility model purpose adopts is: a kind of liquid-liquid-liquid three phase extraction apparatus, at least comprise sample bottle and bottle stopper, bottle stopper is positioned at the bottle mouth position of sample bottle, has aperture in the bottle stopper, be plugged with interpolation pipe in the aperture, the top of interpolation pipe is connected with sample bottle by aperture.
The bottom internal diameter of described interpolation pipe is greater than the top internal diameter.
Described sample bottle is the plain reagent bottle of penicillium communne or other vial, and magneton is housed in the sample bottle.
The interpolation pipe mouth of pipe is filled in up in the aperture of sample bottle bottle stopper, packed into successively in the interpolation pipe bottom and accept phase (third phase), organic extractant (second phase) and sample solution (first mutually).Splendid attire sample solution in sample bottle is put into the stirring magneton, and the bottle stopper that will have interpolation pipe is filled in the sample bottle that fills sample solution and magneton, and the sample bottle side direction is placed on the magnetic stirring apparatus, stirs, extracts.
Wherein used interpolation pipe is that the bottom internal diameter is less, the interpolation pipe that the top internal diameter is bigger, the buffering empennage is loaded onto in the interpolation pipe bottom, the buffering empennage is the plastics empennage that buffer capacity is arranged, have the interpolation pipe that cushions empennage and can place auto injection bottle splendid attire solvent, the effect of the interpolation pipe of band buffering empennage has two: the one, and to accept phase (third phase) more stable because its less internal diameter in bottom can make, and can strengthen mixing speed like this; The 2nd, can make auto injection complete by the buffering empennage.The size of buffering empennage and the size of size interpolation pipe bottom match, the size of the size of interpolation pipe and auto injection bottle is suitable.
The beneficial effects of the utility model:
1, replaces micro syringe needle point and expensive hollow-fibre membrane with inexpensive interpolation pipe.It is big that interpolation pipe stores the extractant volume, and extraction quantity increases than traditional liquid-liquid-liquid three phase extractions, and extraction efficiency height, organic solvent consumption are little.In addition, analysis cost reduces greatly.
2, the disposable use of interpolation pipe, no cross pollution.
3, accept phase (third phase) and be placed on the influence that is not subjected to gravity and buoyancy in the interpolation pipe, then the solvent types range of choice is expanded greatly.More stable then mixing speed can improve greatly owing to accept mutually in addition, reaches balance time thereby greatly shorten.
Description of drawings
The present invention is further illustrated to engage drawings and Examples below.
Fig. 1 is a structural representation of the present utility model.
Fig. 2 is the state diagram of the utility model auto injection.
Among the figure: 1. interpolation pipe, 2. bottle stopper, 3. sample bottle, 4. magnetic stirring apparatus, 5. magneton, 6. bubble, 7. sample solution (first phase) is 8. accepted phase (third phase), 9. organic facies (second phase), 10. buffering empennage, 11. auto injection bottles.
The specific embodiment
The novel liquid-liquid-liquid that provides three phase extraction apparatus of this use as shown in Figure 1, at least comprise sample bottle 3, bottle stopper 2, bottle stopper 2 is positioned at the bottle mouth position of sample bottle 3, has aperture in the bottle stopper 2, be plugged with interpolation pipe 1 in the aperture, the top of interpolation pipe 1 is connected with sample bottle 3 by aperture.Interpolation pipe 1 mouth of pipe is filled in the aperture of bottle stopper 2 of sample bottle 3 up, and 8.0 microlitres of packing into successively in interpolation pipe 1 bottom are accepted phase (third phase) 8,7.0 microlitre organic extractants (second phase) 9 and an amount of sample solution (first mutually) 7; Magneton 5 is put in splendid attire sample solution and acid in sample bottle 3.The bottle stopper 2 that is plugged with interpolation pipe 1 is filled in the sample bottle 3 that fills sample and magneton 5, then sample bottle 3 side direction are placed on the magnetic stirring apparatus 4, stir, extract.
Utilize the utility model to measure four kinds of phenolic compounds in the refuse landfill sewage.
8.0 microlitres of packing into successively in interpolation pipe 1 bottom accept phase (third phase: concentrated ammonia liquor), 7.0 microlitre organic extractants (second phase) and an amount of sample solution (first mutually), interpolation pipe 1 mouth of pipe is filled in up in the aperture of bottle stopper 2 of sample bottle 3; In sample bottle, adorn 8.0 milliliter of 30 mcg/ml sample (phenol, catechol, resorcinol, hydroquinones) solution, 16.0 microlitre SPA, put into the stirring magneton, the bottle stopper 2 that will have interpolation pipe 1 is then filled in the sample bottle 3 that fills sample and magneton 5, sample bottle 3 side direction are placed on the magnetic stirring apparatus 4, stir, behind the extraction 10min, two-phase above taking out adds the dense formic acid of 5.0 microlitres at concentrated ammonia liquor in mutually and neutralizes, put buffering empennage 10 then as shown in Figure 2, will have the interpolation pipe 1 that cushion empennage 10 and put auto injection bottle 11 into and advance HPLC and separate detection.
Chromatographic condition: chromatographic column: Essil ODS C
18(150 * 4.6 millimeters); Phase flows: methyl alcohol: water=10: 90 (volume: volume); Flow velocity: 1 ml/min; Detect wavelength: 274 nanometers.
Its result compares with conventional liquid-liquid-liquid three phase extractions, and the 11-47 of conventional liquid-liquid-liquid three phase extraction apparatus that this use is novel to be doubly.And being applied to the mensuration of four kinds of phenolic compounds in the actual refuse landfill sewage, the rate of recovery is between 82.2-108%.And interpolation pipe, buffering empennage, auto injection bottle that this law is used all are the common things in market.Liquid-liquid-liquid three phase extraction apparatus that the utility model provides, simple, the easy row of method of operating, the extraction efficiency height is very suitable for complicated biology, the extraction of environmental sample, enrichment.
Claims (4)
1. liquid-liquid-liquid three phase extraction apparatus comprise sample bottle and bottle stopper at least, and bottle stopper is positioned at the bottle mouth position of sample bottle, it is characterized in that: have aperture in the bottle stopper, be plugged with interpolation pipe in the aperture, the top of interpolation pipe is connected with sample bottle by aperture.
2. liquid-liquid-liquid three phase extraction apparatus according to claim 1 is characterized in that: the top internal diameter of interpolation pipe is greater than the bottom internal diameter.
3. liquid-liquid-liquid three phase extraction apparatus according to claim 1, it is characterized in that: sample bottle is a vial, and is provided with magneton in the sample bottle.
4. liquid-liquid-liquid three phase extraction apparatus according to claim 1, it is characterized in that: the sample bottle side direction places on the magnetic stirring apparatus, stirs, extracts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007200882411U CN201168460Y (en) | 2007-11-16 | 2007-11-16 | Liquor-liquor-liquor three-phase extraction plant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNU2007200882411U CN201168460Y (en) | 2007-11-16 | 2007-11-16 | Liquor-liquor-liquor three-phase extraction plant |
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| Publication Number | Publication Date |
|---|---|
| CN201168460Y true CN201168460Y (en) | 2008-12-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNU2007200882411U Expired - Fee Related CN201168460Y (en) | 2007-11-16 | 2007-11-16 | Liquor-liquor-liquor three-phase extraction plant |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102294129A (en) * | 2011-03-02 | 2011-12-28 | 中国科学院过程工程研究所 | Three-phase extraction tank |
| CN103768950A (en) * | 2014-01-13 | 2014-05-07 | 大连海事大学 | Membrane extraction device and membrane extraction method based on microporous polymeric membrane |
| CN104857741A (en) * | 2015-05-19 | 2015-08-26 | 上海化工研究院 | Valveless liquid-liquid extraction device |
| CN105784455A (en) * | 2016-05-16 | 2016-07-20 | 张起香 | Extraction structure and liquid pretreatment device |
-
2007
- 2007-11-16 CN CNU2007200882411U patent/CN201168460Y/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102294129A (en) * | 2011-03-02 | 2011-12-28 | 中国科学院过程工程研究所 | Three-phase extraction tank |
| CN102294129B (en) * | 2011-03-02 | 2013-10-16 | 中国科学院过程工程研究所 | Three-phase extraction tank |
| CN103768950A (en) * | 2014-01-13 | 2014-05-07 | 大连海事大学 | Membrane extraction device and membrane extraction method based on microporous polymeric membrane |
| CN103768950B (en) * | 2014-01-13 | 2016-01-13 | 大连海事大学 | A kind of membrane extraction device based on microporous polymer film and membrane extraction method |
| CN104857741A (en) * | 2015-05-19 | 2015-08-26 | 上海化工研究院 | Valveless liquid-liquid extraction device |
| CN105784455A (en) * | 2016-05-16 | 2016-07-20 | 张起香 | Extraction structure and liquid pretreatment device |
| CN105784455B (en) * | 2016-05-16 | 2018-08-17 | 张起香 | Extract structure and liquid preprocessing device |
| US10150065B2 (en) | 2016-05-16 | 2018-12-11 | Tianjin Anbang Jinahe Technology Co., Ltd. | Extraction structure, extraction module, and liquid pretreatment device |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081224 Termination date: 20091216 |