CN101406766B - Ion liquid multiple-dropping liquid-phase microextraction device and use method - Google Patents
Ion liquid multiple-dropping liquid-phase microextraction device and use method Download PDFInfo
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- CN101406766B CN101406766B CN2008100720685A CN200810072068A CN101406766B CN 101406766 B CN101406766 B CN 101406766B CN 2008100720685 A CN2008100720685 A CN 2008100720685A CN 200810072068 A CN200810072068 A CN 200810072068A CN 101406766 B CN101406766 B CN 101406766B
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Abstract
The invention provides a device for multi-drip liquid-phase micro-extraction of ion liquid and a method for using the same. The device comprises an extraction flask provided with a sealed flask cap, a liquid-phase micro-extraction injector, a multi-hole extracting head, a stirrer, and a bracket. When the device is used, the lower end of the liquid-phase micro-extraction injector passes through the sealed flask cap of the extraction flask and extends into solution to be extracted to perform extraction. The device has the advantages of simple structure, reasonable design, easy production, easy and convenient operation, small dead volume, easy cleaning, reusability, and high enriching efficiency; besides, the device is convenient to use together with various analytical instruments, can control and improve the volume of an extraction solvent conveniently, filter the ionic liquid after the extraction, ensure the cleanness of a sample solvent, and avoid the pollution to a chromatographic column, and is applicable to the enrichment and the extraction of a trace amount of organic substances in various complex samples.
Description
Technical field
The invention belongs to the analytical chemistry field, more specifically relate to a kind of device and using method that is used for ion liquid multiple-dropping liquid-phase microextraction.
Background technology
(liquid-phase microextraction LPME) as a kind of novel sample pre-treatments technology, was proposed and development by Jeannot and Cantwell in 1996 liquid-phase micro-extraction.This technology centralized procurement sample, extract and concentrate in one, highly sensitive, simple to operate, but also have characteristics such as quick, cheapness.In addition, required organic solvent only is a few microlitre to tens microlitres, is an eco-friendly sample pre-treatments new technology, is particularly suitable for the mensuration of trace in the environmental sample, ultra trace pollutant.
Ionic liquid at room temperature is a kind of a kind of salt that is mutually combined and formed by organic cation and inorganic anion, and fusing point is usually about below 100 ℃, the material that is in a liquid state under the room temperature.As a kind of solvent, ionic liquid at room temperature has the incomparable advantage of a lot of other organic solvents and unique character: 1. can be by designing ion liquid yin, yang ion part to reach needed certain specific character; 2. almost do not have vapour pressure, non-volatile, nonflammable, be difficult for oxidation, adjustable viscosity, good heat endurance; 3. water and air is stablized, is convenient to operational processes, is easy to reclaim; 4. many organic compounds and metal ion are all had fine solubility, the two-phase system of can provide-individual non-water, polarity is adjustable can be used as the non-molten altogether of a water and uses mutually in chemical separation process, or the like.In recent years, ionic liquid had become one of research focus of analytical chemistry aspect.In view of ionic liquid at room temperature has solvability preferably to many organic compounds, and extremely low vapour pressure (volatilization hardly) is arranged, and the solubility in water is less, has bigger viscosity and density, can obtain bigger suspension droplet size again, thereby improve mensuration sensitivity.Thereby ionic liquid at room temperature is a kind of desirable liquid-phase micro-extraction solvent.
Present existing hanging drop liquid-phase micro-extraction method comprises two kinds of extracting process of head space list dropping liquid-phase microextraction and immersion liquid-phase micro-extraction.The organic solvent that these two kinds of methods are used is some volatile solvents normally, and viscosity is less, or just on the extraction pinhead sleeve polyfluortetraethylene pipe to increase the extractant volume.Limited droplet size has restricted loading capacity, and the effumability of solvent is restricted the extraction time and influence experiment precision, thereby has influenced the extraction results of whole experiment.
Also have the people that the slightly solubility ionic liquid is used for single dropping liquid-phase microextraction method, but the ion liquid abstraction liquid that this method is effectively utilized is long-pending little, effect of extracting can't improve.
Goal of the invention
The purpose of this invention is to provide a kind of device and using method that is used for ion liquid multiple-dropping liquid-phase microextraction; This apparatus structure is simple, and is reasonable in design, makes easily, easy and simple to handle, dead volume is little, is easy to clean, reusable, the bioaccumulation efficiency height is convenient to and various analytical instrument couplings, can easily control the volume that improves extractant, and can the ionic liquid after the extraction be filtered, guarantee the cleaning of sample introduction solvent, avoid pollution chromatographic column, and applicable to the enrichment and the extraction of trace organic substance in the various complex samples.
The device of ion liquid multiple-dropping liquid-phase microextraction of the present invention, comprise the extraction flask and the liquid-phase micro-extraction syringe that have seal bottle cap, the lower end of described liquid-phase micro-extraction syringe is passed seal bottle cap and is stretched in the extraction flask, and the lower end of described liquid-phase micro-extraction syringe is connected with the porous extracting head; Described porous extracting head comprises a cavity, and cavity one end is for connecting the liquid-phase micro-extraction injector end; Cavity other end opening part is the porous bottom, also is provided with the organic filter membrane that is parallel to the porous bottom in the described cavity; Also be provided with agitating device on the described extraction flask.
The using method of ion liquid multiple-dropping liquid-phase microextraction device of the present invention is:
A) earlier with in the ionic liquid inhalant liquid phase extraction syringe;
B) liquid-phase micro-extraction syringe front end is passed the seal bottle cap of extraction flask;
C) the porous extracting head is connected the described liquid-phase micro-extraction syringe of step 1, and guarantees the no leakage of interface sealing;
D) the liquid-phase micro-extraction syringe insertion that will be with the porous extracting head is treated in the extraction solution, depress injector push-rod slowly, ionic liquid is entered in the cavity of porous extracting head, ionic liquid passes through organic filter membrane behind the gas in the row's for the treatment of optical cavity body under the effect of pressure, from the pore of porous bottom, become droplet-like to be extruded, and owing to the tension force effect is suspended on the bottom;
E) in extraction flask the extraction certain hour after, draw back ionic liquid slowly, ionic liquid filtered the interference of removal impurity and eliminated bubble through organic filter membrane of porous extracting head this moment, after treating that the interior ionic liquid of porous extracting head sucks back the liquid-phase micro-extraction syringe fully, open the extraction flask bottle cap, shed the porous extracting head, Extract phase extraction syringe, sample solution can be used for analyzing.
Remarkable advantage of the present invention is:
1) special construction of apparatus of the present invention, its dead volume is little, can effectively reduce the dilute strength of extract; Organic filter membrane can be used for filtering the impurity of introducing the extraction back and eliminating bubble; Many pores are arranged at the porous plastics bottom, can be used to hang the ion drop, thereby increase the cumulative volume of drop, increase extraction quantity.
2) the present invention adopts ionic liquid as extractant, because its special physical property and the bottom that hangs on micro-extraction device that can be more, more lasting effectively raises effect of extracting.
3) porous of the present invention bottom has increased the extractant cumulative volume of present single dropping liquid-phase microextraction greatly, guarantees bigger extraction volume and extracting power;
4) organic filter membrane of device of the present invention can be removed impurity such as big molecule after filtering extraction, and can eliminate the interference of bubble, solvent after organic filter membrane of disposal type effectively guarantees to extract is clean, avoid the pollution of sample introduction solvent and the problem that big molecule disturbs, guaranteed the pollution that is not subjected to complex matrices of the analytical system of coupling.
5) porous extracting head dead volume of the present invention is little, is easy to clean, and is reusable;
6) each parts of device of the present invention can freely split, replace, and the convenience that has guaranteed device maintenance and assembling is with quick.
7) device of the present invention not only keeps traditional single dropping liquid-phase microextraction to integrate the advantage of separation, enrichment and sample introduction, but also on single dropping liquid-phase microextraction basis, can increase the stability of volume, raising extraction efficiency and the drop of extraction liquids greatly.This device is convenient to and various analytical instrument couplings, can easily control the volume that improves extractant, and can the ionic liquid after the extraction be filtered, guaranteed the cleaning of sample introduction solvent, thereby avoided pollution, and applicable to the enrichment and the extraction of trace organic substance in the various complex samples to chromatographic column.
Description of drawings
Fig. 1 is the porous extracting head schematic diagram of ion liquid multiple-dropping liquid-phase microextraction device of the present invention, wherein, and 1 porous extracting head; 2 organic filter membranes; 3 porous bottom.
Fig. 2 is the porous bottom diagram of the porous extracting head of ion liquid multiple-dropping liquid-phase microextraction device of the present invention.
Fig. 3 is the embodiment of the invention 1 a detachable funnel-form porous extracting head schematic diagram, and wherein 10 for splitting the cavity hatch place.
Fig. 4 is the fractionation upper chamber figure of the porous extracting head of ion liquid multiple-dropping liquid-phase microextraction device of the present invention; Split the cavity hatch place on 4.
Fig. 5 is the fractionation lower cavity figure of the porous extracting head of ion liquid multiple-dropping liquid-phase microextraction device of the present invention.Split the cavity hatch place 5 times.
Fig. 6 is the sealing device schematic diagram of the whole device of many drops of ionic liquid ionic liquid liquid-phase micro-extraction.Wherein, 6 liquid-phase micro-extraction syringes; 7 have the extraction flask of seal bottle cap; 8 controllable temperature magnetic stirring apparatus; 9 iron stands.
The specific embodiment
The device of ion liquid multiple-dropping liquid-phase microextraction of the present invention, comprise the extraction flask 7 and the liquid-phase micro-extraction syringe 6 that have seal bottle cap, the lower end of described liquid-phase micro-extraction syringe 6 is passed seal bottle cap and is stretched in the extraction flask 7, and the lower end of described liquid-phase micro-extraction syringe 6 is connected with porous extracting head 1; Described porous extracting head 1 comprises a cavity, and cavity one end is for connecting the liquid-phase micro-extraction injector end; Cavity other end opening part is porous bottom 3, also is provided with the organic filter membrane 2 that is parallel to the porous bottom in the described cavity; Also be provided with agitating device 8 on the described extraction flask.
Described liquid-phase micro-extraction syringe is arranged on the support 9; Support can adopt iron stand.
Described agitating device 8 is the controllable temperature magnetic stirring apparatus.
Described porous extracting head cavity can be upper and lower detachable structure; The upper and lower fractionation cavity hatch of porous extracting head place is set to and can fastens mutually, but as is provided with the spiral lamination that can fasten or the snap-fit design of alternate manner.
Described porous extracting head cavity can adopt plastic material for funnel shaped or cylindric etc.
Organic filter membrane is a macromolecular material, can be in polyamide, cellulose acetate, aromatic polyamide, polyether sulfone or the poly-fluoropolymer polymer etc. a kind of.
Assemble device of the present invention according to above structure.
The using method of ion liquid multiple-dropping liquid-phase microextraction device of the present invention is:
A) earlier with in the ionic liquid inhalant liquid phase extraction syringe;
B) liquid-phase micro-extraction syringe front end is passed the seal bottle cap of extraction flask;
C) the porous extracting head is connected the described liquid-phase micro-extraction syringe of step 1, and guarantees the no leakage of interface sealing;
D) the liquid-phase micro-extraction syringe insertion that will be with the porous extracting head is treated in the extraction solution, depress injector push-rod slowly, ionic liquid is entered in the cavity of porous extracting head, ionic liquid passes through organic filter membrane behind the gas in the row's for the treatment of optical cavity body under the effect of pressure, from the pore of porous bottom, become droplet-like to be extruded, and owing to the tension force effect is suspended on the bottom;
E) in extraction flask the extraction certain hour after, draw back ionic liquid slowly, ionic liquid filtered the interference of removal impurity and eliminated bubble through organic filter membrane of porous extracting head this moment, after treating that the interior ionic liquid of porous extracting head sucks back the liquid-phase micro-extraction syringe fully, open the extraction flask bottle cap, shed the porous extracting head, Extract phase extraction syringe, sample solution can be used for analyzing.
Ionic liquid is replaced by other organic extraction solvent as required.
Below be specific embodiments of the invention, but the present invention is not limited only to this.
According to the above device, adopt detachable funnel-form porous extracting head.
Extraction solution of the present invention comprises: extraction matrix (comprises water sample, blood sample, urine sample etc.; The extraction target substance); The extraction conditions regulator solution comprises HCl, NaOH etc.
Ionic liquid of the present invention comprises: 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate etc.Ionic liquid is replaceable to be other organic extraction solvents such as octanol, toluene.
The use step that ion liquid multiple-dropping liquid-phase microextraction device of the present invention extracts is:
1) solution of the required extraction of preparation;
2) in ionic liquid (or other organic extraction solvents) the inhalant liquid phase extraction syringe of elder generation with certain volume (50-100 μ L);
3) liquid-phase micro-extraction syringe lower end is passed the seal bottle cap of extraction flask;
4) porous filter is connected on the described liquid-phase micro-extraction syringe of step 1, and guarantees the no leakage of interface sealing;
5) the liquid-phase micro-extraction syringe insertion that will be with the porous extracting head is treated in the extraction solution, depress injector push-rod slowly, ionic liquid is entered in the cavity body of filtration system, ionic liquid passes through organic filter membrane behind the interior gas of the row's for the treatment of optical cavity under the effect of pressure, from the pore of porous bottom, become droplet-like to be extruded, and owing to the tension force effect is suspended on the bottom;
6) in extraction flask the extraction certain hour after, draw back ionic liquid slowly, ionic liquid filtered through the organic filter membrane in the porous extracting head and removed the impurity interference and eliminate bubble this moment, after treating the complete inhalation syringe of ionic liquid in the porous extracting head cavity, open the extraction flask bottle cap, shed the porous extracting head, Extract phase extraction syringe can liquid phase sample introduction 10-50 μ L.
The step that ion liquid multiple-dropping liquid-phase microextraction device of the present invention cleans is:
1) the porous extracting head is taken off from liquid-phase micro-extraction syringe front end after, the plastic construction of outwarding winding takes out organic filter membrane;
2) filtration system and porous bottom is cleaned with acetone after, change organic filter membrane and get final product.
Claims (10)
1. the device of an ion liquid multiple-dropping liquid-phase microextraction, comprise the extraction flask and the liquid-phase micro-extraction syringe that have seal bottle cap, it is characterized in that: the lower end of described liquid-phase micro-extraction syringe is passed seal bottle cap and is stretched in the extraction flask, and the lower end of described liquid-phase micro-extraction syringe is connected with the porous extracting head; Described porous extracting head comprises a cavity, and cavity one end is for connecting the liquid-phase micro-extraction injector end; Cavity other end opening part is the porous bottom, also is provided with the organic filter membrane that is parallel to the porous bottom in the described cavity; Also be provided with agitating device on the described extraction flask.
2. the device of ion liquid multiple-dropping liquid-phase microextraction according to claim 1, it is characterized in that: described liquid-phase micro-extraction syringe is arranged on the support.
3. the device of ion liquid multiple-dropping liquid-phase microextraction according to claim 1, it is characterized in that: described agitating device is the controllable temperature magnetic stirring apparatus.
4. the device of ion liquid multiple-dropping liquid-phase microextraction according to claim 1, it is characterized in that: described porous extracting head cavity is upper and lower detachable structure.
5. the device of ion liquid multiple-dropping liquid-phase microextraction according to claim 4, it is characterized in that: the upper and lower fractionation cavity hatch of described porous extracting head place is set to and can fastens mutually.
6. the device of ion liquid multiple-dropping liquid-phase microextraction according to claim 5, it is characterized in that: the upper and lower fractionation cavity hatch of described porous extracting head place is provided with the spiral lamination that can fasten.
7. the device of ion liquid multiple-dropping liquid-phase microextraction according to claim 1, it is characterized in that: described porous extracting head cavity is a funnel shaped or cylindric.
8. the device of ion liquid multiple-dropping liquid-phase microextraction according to claim 1 is characterized in that: described organic filter membrane material is a kind of in polyamide, cellulose acetate, polyether sulfone or the poly-fluoropolymer polymer.
9. using method as claim 1,2,3,4,5,6,7 or 8 described ion liquid multiple-dropping liquid-phase microextraction devices, it is characterized in that: the step of described using method is:
A) earlier with in the ionic liquid inhalant liquid phase extraction syringe;
B) liquid-phase micro-extraction syringe front end is passed the seal bottle cap of extraction flask;
C) the porous extracting head is connected the described liquid-phase micro-extraction syringe of step 1, and guarantees the no leakage of interface sealing;
D) the liquid-phase micro-extraction syringe insertion that will be with the porous extracting head is treated in the extraction solution, depress injector push-rod slowly, ionic liquid is entered in the cavity of porous extracting head, ionic liquid passes through organic filter membrane behind the gas in the row's for the treatment of optical cavity body under the effect of pressure, from the pore of porous bottom, become droplet-like to be extruded, and owing to the tension force effect is suspended on the bottom;
E) in extraction flask the extraction certain hour after, draw back ionic liquid slowly, ionic liquid filtered the interference of removal impurity and eliminated bubble through organic filter membrane of porous extracting head this moment, after treating that the interior ionic liquid of porous extracting head sucks back the liquid-phase micro-extraction syringe fully, open the extraction flask bottle cap, shed the porous extracting head, Extract phase extraction syringe, sample solution can be used for analyzing.
10. the using method of ion liquid multiple-dropping liquid-phase microextraction device according to claim 9 is characterized in that: described ionic liquid is replaced by other organic extraction solvent as required.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102512975A (en) * | 2011-12-15 | 2012-06-27 | 江南大学 | Method for preparing hot reversible gel gas separation membrane |
| CN103235066B (en) * | 2013-04-16 | 2014-06-04 | 云南省烟草公司大理州公司 | Hanging drop liquid phase micro-extraction method for extracting aroma component in tobacco leaf |
| CN103293042B (en) * | 2013-06-17 | 2016-01-20 | 山西医科大学 | Filter membrane head space solvent extraction method and device |
| CN103585784B (en) * | 2013-11-15 | 2015-05-20 | 昆明理工大学 | Vortex-aided hollow fiber membrane LPME (liquid-phase micro-extraction) method of steroid hormone |
| CN105910863B (en) * | 2016-04-18 | 2019-08-09 | 佛山盈诺科创投资咨询中心（有限合伙） | A kind of body fluid enrichment smearing machine |
| CN107982958A (en) * | 2017-09-27 | 2018-05-04 | 云南民族大学 | A kind of production method of head space micro-extraction device |
| CN112138428B (en) * | 2020-09-18 | 2021-12-31 | 华中科技大学 | Flat membrane type liquid phase micro-extraction method and application thereof in drug extraction |
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