CN102049150A - Ultrasonic reinforced hollow fiber membrane liquid-phase micro extraction technique and device - Google Patents
Ultrasonic reinforced hollow fiber membrane liquid-phase micro extraction technique and device Download PDFInfo
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- CN102049150A CN102049150A CN2009100710211A CN200910071021A CN102049150A CN 102049150 A CN102049150 A CN 102049150A CN 2009100710211 A CN2009100710211 A CN 2009100710211A CN 200910071021 A CN200910071021 A CN 200910071021A CN 102049150 A CN102049150 A CN 102049150A
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Abstract
The invention relates to an ultrasonic reinforced hollow fiber membrane liquid-phase micro extraction technique and an ultrasonic reinforced hollow fiber membrane liquid-phase micro extraction device. In the technique, proper ultrasonic is applied between sample solution 2 and an extraction phase 4, and the mass transfer process of an analyzed component in each phase is reinforced by using the ultrasonic with adjustable frequency and power so as to quicken the balance of the analyzed component between the phases; and the technique is a novel liquid-phase micro extraction technique. Compared with the conventional liquid-phase micro extraction method, the technique fully reflects the characteristics of quickness and high efficiency on the premise of keeping all advantages of the traditional hollow fiber membrane-based liquid-phase micro extraction technique. The technique belongs to a pretreatment and pre-enrichment technique of multiple analysis means, is a method for measuring liquid phase balance parameters, can be widely applied in many fields of environmental engineering, medicament research and development, food safety and the like, and has strong practical value.
Description
Technical field
The present invention relates under the intensified by ultrasonic wave condition based on hollow-fibre membrane liquid-phase micro-extraction device and application technology thereof, be the pre-treatment and the preenrichment technology of multiple analysis means, also be to measure the balance each other method of parameter of liquid phase, belong to the laboratory applications category.
Background technology
The liquid-phase extraction technology mainly is to utilize compound two differences of solubility in the homophase (for example organic facies and water) not, makes compound reach the process of liquid phase biphase equilibrium under certain condition.But the traditional extraction process exists that volume is big, time-consuming, effort, form problems such as emulsion layer easily, is difficult to satisfy quick balance, highly enriched and requirement that modern analytical technique is microminiaturized; In order to address the above problem, software engineering researchers invent be the liquid-phase micro-extraction device of micro-extraction phase with micro updating drop or liquid film, though this method that is called as the hanging drop type liquid-phase micro-extraction has overcome the problem that the traditional extraction method exists to a certain extent, but, because the micro-extraction in this method is the drop that hangs mutually, deficient in stability has increased difficulty also for operating process and sampling technique, very difficult realization truly fast and efficient; So, in conjunction with the doughnut membrane technology that develops rapidly in recent years, carried out liquid-phase micro-extraction technology based on hollow-fibre membrane, this method utilization has the container of the hollow-fibre membrane of good transparent performance as the micro-extraction phase, both can also play the better protect effect mutually, when having avoided extraneous factor, also greatly reduce the sampling difficulty of liquid-phase micro-extraction technology the influence of micro-extraction phase so that analyte can carry out mass exchange in two liquid phases smoothly to micro-extraction; But the rate of extraction of this liquid-phase micro-extraction technology based on hollow-fibre membrane still is not very desirable, does not still thoroughly realize the quick balance and the efficiently concentrating of operating process, tends to influence subsequent operation.In recent years, the appearance and the development of electric field-enhanced hollow-fibre membrane liquid-phase micro-extraction technology, shortened the extraction time greatly, but because electric field only produces acceleration to charged particle, so this method is not suitable for the preliminary treatment and the analyzing and testing work thereof of non-charging cpd.Recently the ultrasonic emulsification liquid-phase extraction technology that occurs has shortened the extraction time to a certain extent, though can be used for most of organic pre-treatments, complicated operating process, equipment require high, poor stability, have influenced the process of subsequent operation.
Liquid-phase microextraction method mainly contains following several at present: (one) headspace liquid-phase microextraction, method is that micro syringe is placed the container top that sample solution is housed, promoting the micro syringe push rod makes extractant be suspended on the syringe needle below, when sample solution is stirred by magneton in the solution organic matter volatilization enter overhung in the extractant of syringe needle, treat will to analyze behind the extractant inhalation syringe after extraction is finished; (2) based on the hollow-fibre membrane liquid-phase micro-extraction, two ends of U type hollow-fibre membrane are connected on two stainless pins, a pin is used for injecting extraction phase by microsyringe, and another root pin is as the outlet of extraction phase; (3) based on the hollow-fibre membrane liquid-phase micro-extraction, bar-shaped doughnut one end is shut, make microsyringe can insert the fiber core bottom to inject or sucking-off extraction phase solution; (4) based on the hollow-fibre membrane liquid-phase micro-extraction, a bit of hollow-fibre membrane that extraction phase is housed is sealed at both ends, place the sample solution that is stirred fast by magneton, treat that extraction is finished after, the hollow-fibre membrane that extraction phase will be housed takes out analytic sample; (5) based on the hollow-fibre membrane liquid-phase micro-extraction, an end behind the bar-shaped hollow-fibre membrane injection extractant is shut, in film He in the sample solution, respectively put into an electrode, in electric field-enhanced extraction down; (6) extractant and dispersant are added in the sample solution, behind the ultrasonic emulsification, analyze behind the centrifugal extractant that obtains containing object.
In sum, though the liquid-phase micro-extraction technology from having solved the problem that the traditional extraction technology exists to a great extent, its extraction time is also long, generally needs 25-35min, can't really reach requirement fast and efficiently; Though electric field-enhanced liquid-phase micro-extraction makes the extraction time foreshorten to 5-10min greatly, this method only is applicable to the pre-treatment and the analysis thereof of charged compound in sample solution; And ultrasonic emulsification extracting operation process complexity, equipment require high, poor stability.Employing intensified by ultrasonic wave analyte disclosed by the invention mass transfer rate between each liquid phase in based on hollow-fibre membrane liquid-phase micro-extraction technology, can quicken the equilibrium process of analyte greatly in each liquid phase, reach the purpose of quick balance and efficiently concentrating, and can there be problems such as sample discrimination, efficient height, without discrimination.The present invention can be good at and other analytical test means combinations, thereby apparent in the advantage of aspects such as operating cost, detection speed, can be widely used in numerous areas such as environmental project, medicament research and development, food security, has stronger practical value.
Summary of the invention
The invention discloses under a kind of intensified by ultrasonic wave condition based on hollow-fibre membrane liquid-phase micro-extraction device and application technology thereof.The present invention adopts the container of porous hollow fiber membrane as extraction phase, and extraction phase is an organic solvent; The means of strengthening mass transfer are mechanical oscillation and the cavitation that ultrasonic wave causes in sample solution, make the process of balancing each other to finish in a short period of time.Its concrete operating procedure is as follows:
Step 1: hollow-fibre membrane is intercepted suitable length, clean, dry, standby;
Step 2: in the tubular type small container, add an amount of sample solution;
Step 3: the hollow-fibre membrane that will dry places extraction phase solution, and the ultrasonic several seconds is fully immersed in the hollow-fibre membrane hole wall extraction phase solution;
Step 4:, place in the tubular type small container with the hollow-fibre membrane closed at both ends;
Step 5: the probe top that the tubular type small container is placed ultrasonic cleaner;
Step 6: adjust to suitable frequency, power, start ultrasonic separating apparatus, carry out liquid-phase extraction;
Step 7: after reaching extraction equilibrium, from the inner extractant of quantitatively drawing of hollow-fibre membrane, detect with analytical instrument with sampler.
Described hollow-fibre membrane be porous character and have certain support property;
It is 0.5-5mm that described hollow-fibre membrane is preferentially selected internal diameter, and membrane aperture is 0.001-1.0 μ m, and the doughnut membrane material of hole density 10-80%, the intercepted length of hollow-fibre membrane are 2-20cm, and volume is 5-51 μ l;
Described getting is also can use mixed solvent and heterogeneous extraction process by the organic or inorganic solvent mutually;
The frequency of described ultrasonic cleaning machine and the change of power all can influence effect of extracting;
Described intensified by ultrasonic wave extraction adds suitable salt compounds in extraction system can improve the enrichment multiple of organic compound in extractant;
Described intensified by ultrasonic wave extraction adds the support performance that suitable salt compounds can improve hollow-fibre membrane in extraction system.
The present invention is based on the liquid-phase micro-extraction technology of tradition based on hollow-fibre membrane, between sample solution and extraction phase, apply the ultrasonic wave of suitable frequency and power, strengthen the directed mass transport process of analyte in two-phase with mechanical oscillation and cavitation that ultrasonic wave causes in sample solution, thereby reach the purpose of quick balance.This technology is compared with liquid-phase microextraction method in the past, having had concurrently under traditional prerequisite that is had superiority based on the liquid-phase micro-extraction technology of hollow-fibre membrane, has demonstrated fully characteristics fast and efficiently.The present invention is the pre-treatment and the preenrichment technology of multiple analysis means, also is to measure the balance each other method of parameter of liquid phase, can be widely used in numerous areas such as environmental project, medicament research and development, food security, has stronger practical value.
Description of drawings
Fig. 1, intensified by ultrasonic wave hollow-fibre membrane liquid-phase micro-extraction device schematic diagram
Among the figure: 1, the tubular type small container; 2, sample solution; 3, hollow-fibre membrane; 4, extraction phase; 5, ultrasonic probe
Fig. 2, ultrasonic power are to the influence of effect of extracting
Among the figure: 1,30% ultrasonic power; 2,60% ultrasonic powers; 3,90% ultrasonic powers
Fig. 3, intensified by ultrasonic wave are to the influence of effect of extracting
Among the figure: 1, ultrasonic strengthening extraction; 2, the conventional medicament vials extraction; 3 electromagnetic agitation strengthening extractions
The specific embodiment
Further specify technology path of the present invention below in conjunction with drawings and Examples.
Fig. 1 is the intensified by ultrasonic wave hollow-fibre membrane liquid-phase micro-extraction technology of the present invention's proposition and the device schematic diagram of device.The present invention serves as to strengthen driving force with mechanical oscillation and the cavitation that ultrasonic wave causes, the inside mass transfer of forced fluid phase extraction technology increases substantially the efficient based on hollow-fibre membrane liquid-phase micro-extraction technology, makes up liquid-phase micro-extraction device more rapidly and efficiently.
Its concrete operations step comprises:
(1) hollow-fibre membrane is intercepted suitable length, use the absolute ethyl alcohol ultrasonic cleaning, dry for standby;
(2), guarantee that sample solution has the above degree of depth of 2cm to guarantee the abundant contact of two liquid phases with in the pipette adding tubular type small container that analyzed fluid sample solution is quantitative;
(3) the hollow-fibre membrane segment is placed the ultrasonic several seconds of extraction phase solution, make extractant fully infiltrate in the hollow-fibre membrane hole wall after, with film segment closed at both ends;
(4) hollow-fibre membrane is placed the tubular type small container, the tubular type small container is placed on directly over the ultrasonic cleaning machine probe, to guarantee that ultrasonic power density is identical in the sample solution;
(5) regulate ultrasonic wave to suitable frequency and power, open ultrasonic wave and begin the liquid-phase extraction process;
(6) reach extraction equilibrium after,, detect from the inner extractant of quantitatively drawing of hollow-fibre membrane with sampler with gas-chromatography (also can be high pressure liquid chromatography, Capillary Electrophoresis or other analytical instrument).
Embodiment 1: be the influence of probe compound test ultrasonic wave to bioaccumulation efficiency with nitrobenzene
Used film is a hollow-fibre membrane, and the membrane aperture size is 0.02 μ m, fenestra rate 40%, and hollow membrane pipe interior diameter is 1mm.With the n-octyl alcohol is extraction phase, is sample solution with the nitrobenzene dilute aqueous solution.The sample solution of getting 50ml places the ultrasonic several seconds of n-octyl alcohol in the tubular type small container with hollow-fibre membrane, add 25 μ L n-octyl alcohols in the film after, the film closed at both ends is placed in the tubular type small container, the tubular type small container is placed on directly over the ultrasonic cleaning machine probe.Opening power is finished extraction under intensified by ultrasonic wave, with the microsyringe sampling, measure extraction phase and the surplus sample concentration mutually of extraction in gas-chromatography.Fig. 2 is the influence of ultrasonic power to effect of extracting, as seen along with the increase that applies ultrasonic power, equilibration time shortens gradually, but be not that the reinforcement ultrasonic power is high more good more, experiment shows that extractant oozes out in the hollow-fibre membrane if the too high meeting of ultrasonic power causes, influence measurement result, therefore generally taking comparatively moderate ultrasonic power as operand power, is 60% for the desirable ultrasonic power of similar experiment condition, i.e. 180W.
Embodiment 2: electric field-enhanced mass transfer and conventional method effect of extracting are relatively
Be that probe compound is investigated the different of electric field-enhanced mass transfer and traditional stirring means effect of extracting with nitrobenzene, concrete operations are with embodiment 2, just among three groups of contrast experiments first group apply frequency 40kHz, the intensified by ultrasonic wave of power 180W; Second group does not add intensified by ultrasonic wave, but adopts traditional fask oscillating method; The 3rd group does not apply intensified by ultrasonic wave, and the method to apply magnetic agitation that changes is strengthened.Fig. 3 is the influence of intensified by ultrasonic wave to effect of extracting, and experimental result finds that the logP value that three group of methods record is identical, but equilibration time is respectively 15min, 40min and 35min.The present invention's characteristics have rapidly and efficiently been confirmed.
Embodiment 3: the logP that measures pure organic compound with this device
Getting aniline, nitrobenzene, toluene respectively is probe compound, measures the n-octyl alcohol-water partition coefficient of these several pure materials.Method of operating is with embodiment 1, and supersonic frequency is got 40kHz, and power 180W behind the extraction 15min, measures the concentration of analyte at n-octyl alcohol phase and aqueous phase respectively.Calculate n-octyl alcohol phase concentration/aqueous-phase concentration and be distribution coefficient, the logarithm value of distribution coefficient is log P.Log P with several compounds of this device mensuration, see the following form:
Embodiment 4: be used for the environmental water sample Determination of benzene hydrocarbon
The benzene series thing is an important indicator to industrial wastewater and surface water quality monitoring, and this example is the content of benzene series thing in the precise and high efficiency mensuration water sample.From not high at sample concentration, the problem that evaluated error is big has had a strong impact on the accuracy of water quality monitoring when adopting traditional liquid phase chromatography analytical method directly to measure.It is the extraction phase that places hollow-fibre membrane inside that this example still adopts n-octyl alcohol, and sample is in the NaCl aqueous solution of 4mol/L of benzene, toluene, ethylbenzene, isopropylbenzene and cinnamic mixture, behind liquid-phase micro-extraction, measures with gas-chromatography.The experimental implementation of liquid-phase micro-extraction is with embodiment 1, supersonic frequency is got 40kHz, power 180W, extraction time 15min, carrying out measurement result behind the liquid-phase micro-extraction shows, the present invention respectively is 101,205,510,500,600 times for benzene, toluene, ethylbenzene, isopropylbenzene and cinnamic mensuration enrichment multiple in the environmental water sample, has improved the detectability that the benzene series quality testing is surveyed on the basis of extraction fast greatly.
Embodiment 5: the mensuration of residual carbamate chemicals for agriculture in the food
Carbamate chemicals for agriculture is widely used in the agricultural production because of various pests there being good insecticidal effect.Wherein highly toxic furans pellet, Mobucin etc. are often misused in the production of vegetables, fruit, its residual health that has a strong impact on.Gas-chromatography (GC) is the Analytical Techniques of Pesticide Residues of using always, but the carbamate chemicals for agriculture of volatility difference is difficult to directly measure with gas chromatography.It is the extraction phase that places hollow-fibre membrane inside that this example still adopts n-octyl alcohol, and the NaCl aqueous solution that furans pellet, Aldicarb are dissolved in 4mol/L carries out ultrasonic strengthening extraction.The experimental implementation of liquid-phase micro-extraction is with embodiment 1, and supersonic frequency is got 40kHz, power 180W, extraction time 15min, carry out measurement result behind the liquid-phase micro-extraction and show that the present invention can reach 150 times more than for the bioaccumulation efficiency of furans pellet, Mobucin, impurity peaks seldom in the chromatogram.
Embodiment 6: be used for the concentration effect test of drug component at biological sample
Barbital is one of the main medicine with antondin parenteral solution of antipyretic-antalgic, is not having abuse under the situation of physician guidance can cause the generation of malpractice.Because the ubiquity of illegal practice of medicine and some lawless person's overdoses use to reach illegal objective, make this class medicine become poisonous substance common in the judicial expertise simultaneously, and be the trend that rises year by year.In criminal technique was analyzed, because the sample of censorship is generally urine or blood sample, so liquid-liquid extraction was the main extracting method of such medicine.But traditional liquid-liquid extraction length consuming time, solvent-oil ratio is big, and processing procedure is loaded down with trivial details, and extraction process uses a large amount of solvents environment to be polluted and makes operating personnel come to harm.It is the extraction phase that places hollow-fibre membrane inside that this example still adopts n-octyl alcohol, and the NaCl aqueous solution that barbital is dissolved in 4mol/L carries out ultrasonic strengthening extraction.The experimental implementation of liquid-phase micro-extraction is with embodiment 1, supersonic frequency is got 40kHz, power 180W, extraction time 15min, carrying out measurement result behind the liquid-phase micro-extraction shows, the present invention can reach 30 times more than for the bioaccumulation efficiency of barbital, has realized barbital trace, enrichment fast, accurately and detection.
Claims (6)
1. intensified by ultrasonic wave hollow-fibre membrane liquid-phase micro-extraction technology and device, it is characterized in that intensified by ultrasonic wave mass transfer technology is introduced traditional liquid-phase micro-extraction device, with the mass transport process between each liquid phase of intensified by ultrasonic wave liquid-phase micro-extraction technology, can increase substantially efficient based on hollow-fibre membrane liquid-phase micro-extraction technology, and this invention is easy to realize high flux and automation, be liquid-phase micro-extraction device more rapidly and efficiently, its concrete operating procedure is as follows:
Step 1: hollow-fibre membrane is intercepted suitable length, clean, dry, standby;
Step 2: in the tubular type small container, add an amount of sample solution;
Step 3: the hollow-fibre membrane that will dry places extraction phase solution, and the ultrasonic several seconds is fully immersed in the hollow-fibre membrane hole wall extraction phase solution;
Step 4:, place in the tubular type small container with the hollow-fibre membrane closed at both ends;
Step 5: the probe top that the tubular type small container is placed ultrasonic cleaner;
Step 6: adjust to suitable frequency, power, start ultrasonic separating apparatus, carry out liquid-phase extraction;
Step 7: after reaching extraction equilibrium, from the inner extractant of quantitatively drawing of hollow-fibre membrane, detect with analytical instrument with sampler.
2. by the described intensified by ultrasonic wave hollow-fibre membrane of claim 1 liquid-phase micro-extraction technology and device, it is characterized in that, hollow-fibre membrane be porous character and have certain support performance.
3. preferentially selecting internal diameter by the described hollow-fibre membrane of claim 2 is 0.5-5mm, and membrane aperture is 0.001-1.0 μ m, and the doughnut membrane material of hole density 10-80%, the intercepted length of hollow-fibre membrane are 2-20cm, and volume is 5-50 μ l.
4. by the described intensified by ultrasonic wave hollow-fibre membrane of claim 1 liquid-phase micro-extraction technology and device, it is characterized in that extraction phase is the organic or inorganic solvent, also can use mixed solvent and heterogeneous extraction process.
5. by the described intensified by ultrasonic wave hollow-fibre membrane of claim 1 liquid-phase micro-extraction technology and device, it is characterized in that, in extraction system, add suitable salt compounds and can improve the enrichment multiple of organic compound in extractant.
6. by the described intensified by ultrasonic wave hollow-fibre membrane of claim 1 liquid-phase micro-extraction technology and device, it is characterized in that, in extraction system, add the support performance that suitable salt compounds can improve hollow-fibre membrane.
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Cited By (5)
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| CN102607890A (en) * | 2012-03-19 | 2012-07-25 | 泰州市升拓精密仪器有限公司 | Standard sampling device |
| CN102735570A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院宁波材料技术与工程研究所 | Method for determining finisher content in PAN precursor |
| ES2482770A1 (en) * | 2013-01-31 | 2014-08-04 | Universidad De Cádiz | Thermostatic liquid phase microextraction bars for the preconcentration of metallic species (Machine-translation by Google Translate, not legally binding) |
| CN105023569A (en) * | 2015-07-29 | 2015-11-04 | 武汉理工大学 | Resonant frequency adjusting device of ultrasonic system and adjusting method |
| CN107589186A (en) * | 2017-08-30 | 2018-01-16 | 浙江清华长三角研究院 | One kind power-up membrane extraction device and its application method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102607890A (en) * | 2012-03-19 | 2012-07-25 | 泰州市升拓精密仪器有限公司 | Standard sampling device |
| CN102607890B (en) * | 2012-03-19 | 2014-02-19 | 泰州市升拓精密仪器有限公司 | Standard sampling device |
| CN102735570A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院宁波材料技术与工程研究所 | Method for determining finisher content in PAN precursor |
| ES2482770A1 (en) * | 2013-01-31 | 2014-08-04 | Universidad De Cádiz | Thermostatic liquid phase microextraction bars for the preconcentration of metallic species (Machine-translation by Google Translate, not legally binding) |
| CN105023569A (en) * | 2015-07-29 | 2015-11-04 | 武汉理工大学 | Resonant frequency adjusting device of ultrasonic system and adjusting method |
| CN105023569B (en) * | 2015-07-29 | 2018-06-08 | 武汉理工大学 | A kind of regulating device and adjusting method of ultrasonic system resonant frequency |
| CN107589186A (en) * | 2017-08-30 | 2018-01-16 | 浙江清华长三角研究院 | One kind power-up membrane extraction device and its application method |
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Application publication date: 20110511 |