CN101915695A - Centrifuge tube and method for micro-extraction of dispersion liquid - Google Patents
Centrifuge tube and method for micro-extraction of dispersion liquid Download PDFInfo
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- CN101915695A CN101915695A CN 201010250527 CN201010250527A CN101915695A CN 101915695 A CN101915695 A CN 101915695A CN 201010250527 CN201010250527 CN 201010250527 CN 201010250527 A CN201010250527 A CN 201010250527A CN 101915695 A CN101915695 A CN 101915695A
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Abstract
The invention relates to a centrifugal tube for micro-extraction of dispersion liquid. An orifice part which has a slender structure is formed in such a manner that a pipe wall extends to an upper end in an inwardly-concave circular arc form; the length of the slender orifice part is between 0.3 and 0.8 centimeters; and the inner diameter of the orifice at a front end is between 1 and 2 millimeters. A method for micro-extraction by using the centrifugal tube comprises the following steps of: adding 10 ml of water sample into the centrifugal tube; adding a solvent into the centrifugal tube and mixing the solvent and the water sample to form mixed solution; sealing the orifice of the centrifugal tube and rotating the orifice at a speed of 4,000 rpm by using equipment, so that the mixed solution is clarified and an extraction solvent floats on the top surface of the mixed solution; adding 1 ml of purified water into the centrifugal tube to lift the extraction solvent at the position of the orifice; and collecting the extraction solvent by using a chromatogram sample needle and putting the collected extraction solvent into a chromatographic apparatus for analyzing. The disadvantage that only a solvent of which the density is higher than that of water can be used in the conventional device for micro-extraction of the dispersion liquid is overcome.
Description
Technical field
The present invention relates to a kind of liquid-phase micro-extraction device, especially a kind of centrifuge tube and extracting process thereof that is used for dispersive liquid-liquid microextraction.
Background technology
Dispersion liquid phase extraction technology (dispersive liquid-liquid microextraction, DLLME) be a kind of novel sample-pretreating method, compare with existing liquid-liquid extraction, DLLME only needs extraction solvent seldom, greatly reduces the use amount of organic solvent.It (generally is acetonitrile that DLLME is dissolved into spreading agent by the extraction solvent with trace, acetone or methyl alcohol) in, then mixed solvent is added to the water and forms the emulsion system of a kind of water/spreading agent/extraction solvent, or by adopting whirlpool or ultrasonic auxiliary method that extraction solvent is distributed in the aqueous solution after extraction solvent is added to the water, extraction solvent is distributed in the water with minimum drop form, thereby greatly enlarged the contact area between water and the extraction solvent, analyte can be very fast by being extracted in the water in the extraction solvent, at last by the centrifugal bottom that extraction solvent is deposited to centrifuge tube.But existing DLLME also has some shortcomings, the extraction solvent that DLLME uses requires density greater than water, this has limited the choice of Solvent scope greatly, have only some halogen-containing solvents to use, as organochlorine solvents such as chlorobenzene, zellons, but these organochlorine solvents and some analytical instrument are incompatible, and as electron capture detector, and toxicity is also very high.In the present invention, we have developed a kind of novel glass centrifuge tube, adopt than the little organic solvent of water-mass density as extraction solvent, and it is few to have overcome the extraction solvent kind of using in the existing DLLME technology, the shortcoming that toxicity is high, this aspect can be used for the DLLME technology as sample-pretreating method.
Summary of the invention
At the weak point that exists in the problems referred to above, the invention provides a kind of can the use than the little organic solvent of water-mass density, thereby enlarged the centrifuge tube that is used for dispersive liquid-liquid microextraction and the extracting process thereof of DLLME The Application of Technology scope greatly as extraction solvent.
For achieving the above object, the invention provides a kind of centrifuge tube that is used for dispersive liquid-liquid microextraction, the centrifuge tube body is made of body and opening part, and described opening part is the inner concavity circular arc by tube wall and extends to form to the upper end, and described opening part is the elongate structure.
The volume of described centrifuge tube body is 10～12ml, and length (L) is 12cm.
The length L ` of described elongate opening part is 0.3～0.8cm, and the internal diameter a of its front end mouth of pipe is 1～2mm.
The present invention also provides a kind of extracting process that is used for the centrifuge tube of dispersive liquid-liquid microextraction simultaneously, and concrete steps are as follows:
A, will be in the centrifuge tube add the water sample of 10ml;
B, solvent joined in the centrifuge tube mix the back with water sample and form mixed solution;
Behind c, the ferrule with centrifuge tube, rotate under the condition of 4000rpm by equipment, make the mixed solution clarification that becomes, this moment, extraction solvent can float over the top surface of mixed solution;
D, in centrifuge tube, add the pure water of 1ml, make extraction solvent be promoted to the position of the mouth of pipe;
E, collect extraction solvent, and put into chromatographic apparatus analysis by chromatogram sample pin.
Compared with prior art, the present invention has the following advantages:
The invention provides a kind of centrifuge tube that is used for dispersive liquid-liquid microextraction, the volume of centrifuge tube body is 10～12ml, length is 12cm, its opening part is the inner concavity circular arc by tube wall and extends to form to the upper end, opening part is the elongate structure, the length of this elongate opening part is 0.3～0.8cm, and the internal diameter of its front end mouth of pipe is 1～2mm.The extracting process of implementing above-mentioned centrifuge tube is: will add the water sample of 10ml in the centrifuge tube; Solvent joined in the centrifuge tube mix the back with water sample and form mixed solution; Behind the ferrule with centrifuge tube, rotate under the condition of 4000rpm by equipment, make the mixed solution clarification that becomes, this moment, extraction solvent can float over the top surface of mixed solution; In centrifuge tube, add the pure water of 1ml, make extraction solvent be promoted to the position of the mouth of pipe; Collect extraction solvent by chromatogram sample pin, and put into chromatographic apparatus analysis.The present invention is stuporous simple, easy to use, with low cost, has overcome in the existing dispersion liquid micro-extraction device to use the shortcoming of density greater than the solvent of water.The present invention is applicable to organic extraction and collection in the complex matrices samples such as agricultural environment, food security, biochemical analysis.
Description of drawings
Fig. 1 is a structural drawing of the present invention;
Fig. 2 is the cut-open view of Fig. 1;
Fig. 3 is the structural drawing of opening part among Fig. 1.
The main element symbol description is as follows:
1 centrifuge tube body, 2 bodys
3 opening parts
Embodiment
As shown in Figure 1 to Figure 3, the invention provides a kind of centrifuge tube that is used for dispersive liquid-liquid microextraction, the volume of centrifuge tube body 1 is 10～12ml, length L is 12cm, centrifuge tube body 1 is made of body 2 and opening part 3, opening part 3 is the inner concavity circular arc by tube wall and extends to form to the upper end, and opening part 3 is the elongate structure.The length L ` of elongate opening part is 0.3～0.8cm, and the internal diameter of its front end mouth of pipe 3 is a1～2mm.
The present invention also provides a kind of extracting process that is used for the centrifuge tube of dispersive liquid-liquid microextraction, and concrete steps are as follows:
A, will be in the centrifuge tube add the water sample of 10ml;
B, solvent joined in the centrifuge tube mix the back with water sample and form mixed solution;
Behind c, the ferrule with centrifuge tube, rotate under the condition of 4000rpm by equipment, make the mixed solution clarification that becomes, this moment, extraction solvent can float over the top surface of mixed solution;
D, in centrifuge tube, add the pure water of 1ml, make extraction solvent be promoted to the position of the mouth of pipe;
E, collect extraction solvent, and put into chromatographic apparatus analysis by chromatogram sample pin.
The present invention also provides a kind of extracting process that is used for the centrifuge tube of dispersive liquid-liquid microextraction, and concrete steps are as follows:
A, will be in the centrifuge tube add the water sample of 10ml;
B, the toluene of 20ul is mixed with the acetonitrile of 1ml, and mixed solvent joined in the centrifuge tube with after water sample mixes rock gently, form mixed solution;
Behind c, the ferrule with centrifuge tube, by centrifugation apparatus centrifugal rotation 3 minutes under the condition of 4000rpm, make the mixed solution clarification that becomes, this moment, toluene can float over the top surface of mixed solution;
D, in centrifuge tube, add the pure water of 1ml, make toluene be promoted to the position of the mouth of pipe;
E, collect extraction solvent, and put into chromatographic apparatus analysis by chromatogram sample pin.
In the glass centrifuge tube, add the 10mL water sample, organophosphorus concentration is 0.1ng/mL in the water sample, add 1mL acetonitrile (the extraction solvent toluene that contains 20 microlitres), rock centrifuge tube gently, centrifugal 3min under the 4000rpm condition adds about 1mL pure water then, extraction solvent toluene is risen to the glass capillary mouth place of centrifuge tube, use the gas chromatography sample introduction needle that extraction solvent is taken out at last, the air inlet analysis of hplc.The extraction efficiency that uses this method is gathered multiple between 600-1000 times between 60%-95%.
The present invention also provides a kind of extracting process that is used for the centrifuge tube of dispersive liquid-liquid microextraction, and concrete steps are as follows:
A, will be in the centrifuge tube add the water sample of 10ml;
B, the toluene of 20ul joined in the centrifuge tube with after water sample mixes rock the formation mixed solution gently, by the Vltrasonic device ultrasound procedure after 3～5 minutes, this moment, mixed solution formed dispersed system with mixed solution;
Behind c, the ferrule with centrifuge tube, by centrifugation apparatus centrifugal rotation 5～10 minutes under the condition of 4000rpm, make the mixed solution clarification that becomes, this moment, toluene can float over the top surface of mixed solution;
D, in centrifuge tube, add the pure water of 1ml, make toluene be promoted to the position of the mouth of pipe;
E, collect extraction solvent, and put into chromatographic apparatus analysis by chromatogram sample pin.
In the glass centrifuge tube, add the 10mL water sample, organophosphorus concentration is 0.1ng/mL in the water sample, the extraction solvent toluene that adds 20 microlitres, rock centrifuge tube gently, ultrasonic 3-5min, can form coarse dispersion system this moment, centrifugal 5-10min under the 4000rpm condition then, this moment, system became clarification, extraction solvent toluene floats on the water surface, adds about 1mL pure water then, extraction solvent toluene is risen to the glass capillary mouth place of centrifuge tube, use the gas chromatography sample introduction needle that extraction solvent is taken out at last, the air inlet analysis of hplc.The extraction efficiency that uses this method is gathered multiple between 600-1000 times between 60%-95%.
Only the above person only is preferred embodiment of the present invention, is familiar with the professional person of this skill such as. after understanding technological means of the present invention, natural energy is changed under instruction of the present invention according to the needs of reality.Therefore all equal variation and modifications of being done according to the present patent application claim once should still belong in the scope that patent of the present invention contains.
Claims (6)
1. centrifuge tube that is used for dispersive liquid-liquid microextraction, the centrifuge tube body is made of body and opening part, it is characterized in that, and described opening part is the inner concavity circular arc by tube wall and extends to form to the upper end, and described opening part is the elongate structure.
2. a kind of centrifuge tube that is used for dispersive liquid-liquid microextraction as claimed in claim 1 is characterized in that the volume of described centrifuge tube body is 10～12ml, and length (L) is 12cm.
3. a kind of centrifuge tube that is used for dispersive liquid-liquid microextraction as claimed in claim 1 is characterized in that the length of described elongate opening part (L`) is 0.3～0.8cm, and the internal diameter of its front end mouth of pipe (a) is 1～2mm.
4. a kind of extracting process that is used for the centrifuge tube of dispersive liquid-liquid microextraction as claimed in claim 1 is characterized in that concrete steps are as follows:
A, will be in the centrifuge tube add the water sample of 10ml;
B, solvent joined in the centrifuge tube mix the back with water sample and form mixed solution;
Behind c, the ferrule with centrifuge tube, rotate under the condition of 4000rpm by equipment, make the mixed solution clarification that becomes, this moment, extraction solvent can float over the top surface of mixed solution;
D, in centrifuge tube, add the pure water of 1ml, make extraction solvent be promoted to the position of the mouth of pipe;
E, collect extraction solvent, and put into chromatographic apparatus analysis by chromatogram sample pin.
5. a kind of extracting process that is used for the centrifuge tube of dispersive liquid-liquid microextraction as claimed in claim 4 is characterized in that concrete steps are as follows:
A, will be in the centrifuge tube add the water sample of 10ml;
B, the toluene of 20ul is mixed with the acetonitrile of 1ml, and mixed solvent joined in the centrifuge tube with after water sample mixes rock gently, form mixed solution;
Behind c, the ferrule with centrifuge tube, by centrifugation apparatus centrifugal rotation 3 minutes under the condition of 4000rpm, make the mixed solution clarification that becomes, this moment, toluene can float over the top surface of mixed solution;
D, in centrifuge tube, add the pure water of 1ml, make toluene be promoted to the position of the mouth of pipe;
E, collect extraction solvent, and put into chromatographic apparatus analysis by chromatogram sample pin.
6. a kind of extracting process that is used for the centrifuge tube of dispersive liquid-liquid microextraction as claimed in claim 4 is characterized in that concrete steps are as follows:
A, will be in the centrifuge tube add the water sample of 10ml;
B, the toluene of 20ul joined in the centrifuge tube with after water sample mixes rock the formation mixed solution gently, by the Vltrasonic device ultrasound procedure after 3～5 minutes, this moment, mixed solution formed dispersed system with mixed solution;
Behind c, the ferrule with centrifuge tube, by centrifugation apparatus centrifugal rotation 5～10 minutes under the condition of 4000rpm, make the mixed solution clarification that becomes, this moment, toluene can float over the top surface of mixed solution;
D, in centrifuge tube, add the pure water of 1ml, make toluene be promoted to the position of the mouth of pipe;
E, collect extraction solvent, and put into chromatographic apparatus analysis by chromatogram sample pin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010250527 CN101915695A (en) | 2010-08-11 | 2010-08-11 | Centrifuge tube and method for micro-extraction of dispersion liquid |
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| CN 201010250527 CN101915695A (en) | 2010-08-11 | 2010-08-11 | Centrifuge tube and method for micro-extraction of dispersion liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897456A (en) * | 2015-05-08 | 2015-09-09 | 河北工业大学 | Method for enriching phenol in water by utilizing [C4mim]PF6-TBP binary extractant |
| CN113018904A (en) * | 2021-03-16 | 2021-06-25 | 中国科学院地理科学与资源研究所 | Dispersion liquid-liquid micro-extraction device and method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663662A (en) * | 2004-12-24 | 2005-09-07 | 清华大学 | Hanging drop type liquid-liquid micro-extraction method |
| CN101762417A (en) * | 2010-01-18 | 2010-06-30 | 福州大学 | Dispersive liquid-liquid microextraction method for pretreatment of plant hormone |
-
2010
- 2010-08-11 CN CN 201010250527 patent/CN101915695A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663662A (en) * | 2004-12-24 | 2005-09-07 | 清华大学 | Hanging drop type liquid-liquid micro-extraction method |
| CN101762417A (en) * | 2010-01-18 | 2010-06-30 | 福州大学 | Dispersive liquid-liquid microextraction method for pretreatment of plant hormone |
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of Separation science》 20090930 Mir Ali Farajzadeh et al. Dispersive liquid-liquid microextraction using extraction solvent lighter than water 第32卷, 第18期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897456A (en) * | 2015-05-08 | 2015-09-09 | 河北工业大学 | Method for enriching phenol in water by utilizing [C4mim]PF6-TBP binary extractant |
| CN104897456B (en) * | 2015-05-08 | 2017-07-04 | 河北工业大学 | The method for utilizing [C4mim] PF6 TBP binary extractants that phenol is enriched with from water |
| CN113018904A (en) * | 2021-03-16 | 2021-06-25 | 中国科学院地理科学与资源研究所 | Dispersion liquid-liquid micro-extraction device and method |
| CN113018904B (en) * | 2021-03-16 | 2022-03-01 | 中国科学院地理科学与资源研究所 | Dispersion liquid-liquid micro-extraction device and method |
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Application publication date: 20101215 |