CN103083940A - Microwave-assisted-hollow filter-liquid/liquid micro-extraction device and application - Google Patents
Microwave-assisted-hollow filter-liquid/liquid micro-extraction device and application Download PDFInfo
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- CN103083940A CN103083940A CN2012103685035A CN201210368503A CN103083940A CN 103083940 A CN103083940 A CN 103083940A CN 2012103685035 A CN2012103685035 A CN 2012103685035A CN 201210368503 A CN201210368503 A CN 201210368503A CN 103083940 A CN103083940 A CN 103083940A
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Abstract
The invention relates to a microwave-assisted-hollow filter-liquid/liquid micro-extraction device and an application thereof. At first, a hollow fiber tube with molecular weight cutoff more than a specific molecular weight is selected and cut into small tubes with a proper length; a certain amount of organic solvent is injected, the ends of the hollow fiber tube are sealed and the hollow fiber tube is fixed on silica gel pieces and arranged in a small sample bottle; and a sample phase-supply solution is extracted by using the extraction device. The microwave-assisted-hollow filter-liquid/liquid micro-extraction device provided by the invention synchronously separates, extracts, purifies and enriches a trace amount of target compounds in a complex matrix sample with liquid/liquid micro-extraction combination according to the properties that the pore size of the hollow fiber tube can be used for simply, conveniently and effectively retaining and separating the ineffective bio-macromolecules; and meanwhile, the balance time is reduced in a microwave-assisted combination manner, so that the rapidness and the high efficiency can be realized. The microwave-assisted-hollow filter-liquid/liquid micro-extraction device provided by the invention has the advantages of low preparation cost and easiness of operation, not only is applicable to analysis of a complex sample, such as a biological tissue and a food sample, but also can be applied to separation, extraction and enrichment of trace amount of the target compounds of the sample, and the separation, the purification or the preparation of the bio-molecules.
Description
Technical field
The invention belongs to the chemical analysis instrument field tests, the microwave that relates in particular to highly effective is auxiliary-doughnut-liquid/liquid micro-extraction device, be applicable to extraction, purification, separation and the extracting and enriching of trace target compound in sample that biology, environment, food and medicine etc. have complex matrices.
Background technology
Detection with trace target compound in the complicated substrate sample usually needs to carry out the multistep sample pre-treatments, just can enter instrument analysis.Traditional sample-pretreating method mainly contains SPE, liquid-solid extraction, liquid-liquid extraction, Soxhlet extracting, ultrasonic wave assisted extraction etc., have limitation in various degree, as numerous and diverse in operating process, consuming time, compatibility and poor stability, organic solvent consumption is large, separative efficiency is low etc.In addition, because in the complex matrices sample, often ambient interferences is large and can't measure the target compound of trace concentration.
Doughnut-liquid-phase micro-extraction (Hollow Fiber-Liquid Phase Micro-extraction, HF-LPME) is a kind of novel Sample Pretreatment Technique.HF-LPME is collection extraction, separation, a purifying and the technology that concentrates in one, thereby this technology utilizes the large molecule of micropore restriction of doughnut can not enter extraction phase minimizing matrix interference, and doughnut is that disposable use can be avoided cross-contamination issue, have that the organic solvent consumption is few, purification efficiency is high, simple operating steps, be easy to and the advantages such as other multiple analytical instrument coupling, be widely used in environment, biological sample.But, the extraction efficiency of HF-LPME depends on the solubility of component to be measured in extraction phase, and in existing two phase extraction patterns, analyte enters in extraction phase with absorption or passive diffusion way, not only mass transfer rate is low, equilibration time is long, and analyte can't dissociate out from sample matrices fast.
Microwave auxiliary extraction (Microwave Assisted Extraction, MAE) is a kind of novel Sample Pretreatment Technique that improves the object extraction efficiency by microwave energy.MAE produces a large amount of heat energy that friction and collision brought and the raising of mass transfer velocity with the instantaneous polarization of microcosmic particle under the microwave electromagnetic field action, different material is different to the degree of absorption of microwave energy, be that the microwave alternative heats each component, impel object from Matrix separation, enter into extraction phase, thus quick, the high efficiency extraction of Realization analysis thing.MAE because of have high selectivity, extraction efficiency high, quick, be suitable for the advantages such as determination system of thermal unstable material, usually be applied in the determination processes such as textile, water sample, deposit, soil, Chinese medicine.
Summary of the invention
The purpose of this invention is to provide a kind of efficient, easy microwave assists-doughnut-liquid/liquid micro-extraction device, it can eliminate the interference that large biological molecule, protein and lipid that sample substrate in liquid-phase extraction exists are brought, and improves the doughnut liquid-phase micro-extraction as the mass transfer rate of sample-pretreating method and extracting and enriching efficient, reappearance and the rate of recovery, shortening equilibration time.
The application of another object of the present invention is to provide this kind microwave auxiliary-doughnut-liquid/liquid micro-extraction device.
Operation of the present invention is quick, easy, cost is low, by injecting in the hollow fiber conduit of an existing end closure after a certain amount of organic solvent other end sealing, and be fixed on hollow fiber conduit on silica gel piece and be placed on and form extraction equipment in sample flasket.When hollow fiber conduit being placed in sample for phase solution, giving certain microwave energy on micro-wave oven and stirring a period of time on magnetic stirring apparatus, microwave selective heats each component in sample, promote target compound to separate from sample substrate and utilize the micropore restriction of doughnut greater than the molecule of certain specified molecular weight, target compound enters into extraction phase through the micropore on hollow fiber conduit, extracting and enriching by the organic solvent phase more directly will manage at last interior remaining organic solvent and be drawn to the sample introduction bottle and get final product.Above-mentioned microwave is auxiliary-and doughnut-liquid/liquid-micro-extraction device solved large molecule, protein and part lipid interfering material in complex sample matrix to the impact of trace target compound analysis and avoided the target compound cross-contamination issue.
Above-mentioned microwave is auxiliary-doughnut-liquid/liquid micro-extraction device in, the material of doughnut can be all have pore diameter range at nanoscale to micron-sized microporous hollow fiber pipe.
Above-mentioned microwave is auxiliary-doughnut-liquid/liquid micro-extraction device in, the organic solvent in accepting mutually can be that all have extraction function and the less organic solvent of volatility to target compound.
Description of drawings
Fig. 1 is that microwave of the present invention is assisted-doughnut-liquid/liquid micro-extraction device;
Fig. 2 be milk sample (mark-on concentration is 2 μ g/kg) through microwave auxiliary-doughnut-liquid/liquid micro-extraction device extraction after the MRM figure (liquid chromatography-tandem mass spectrometry analysis) of sample introduction.
The specific embodiment
for improve microwave auxiliary-doughnut-liquid/liquid micro-extraction device is on the impact of the effect of extracting of target compound, effectively utilize hollow fiber conduit to hold back the characteristics of molecule with molecular size range, the enrichment times of raising to target compound, can be optimized from the following aspects: the one, select different organic solvents, with hollow fiber conduit, stronger affinity is arranged as selecting, target compound to be analyzed there is deliquescent organic solvent preferably, can make this solvent be easy to enter in the hole of doughnut tube wall and can keep stablizing and be easy to extract target compound, the 2nd, can by producing a large amount of heat energy, improve the mass transfer rate of target compound in sample by changing microwave power and microwave time, shorten target compound in two alternate equilibration times, improve extraction efficiency, the 3rd, can change the ionic strength that supplies phase in sample solution, by adding some salt (being generally sodium chloride) and hydrone to form hydrated ion, reduced the combination for the treatment of extracting substance and hydrone, make and treat that extracting substance is free in confession mutually more, and then make compound easier of accepting middle transfer the mutually, be that ionic strength has changed the distribution coefficient of compound in supplying phase and accepting mutually, improve the extraction efficiency to target compound, the 4th, can change the mixing speed of magnetic stirring apparatus, constantly update for phase solution by changing the outer sample of hollow fiber conduit, accelerate the mass transport process of target compound, improve extraction efficiency.
Embodiment 1(adopt microwave auxiliary-doughnut-liquid/liquid micro-extraction device measures promise ketone, sulfamido and macrolides totally 27 kinds of Antibiotique compositions in milk sample in conjunction with LC-MS/MS)
Hollow fiber conduit is cut into segment (approximately 5 cm), with methanol/water (ultrasonic cleaning 20 min of v:v=1:1), then use acetone soln ultrasonic cleaning 5 min, after drying, with an end closure, standby with sealing machine.Take sample 15 g (being accurate to 0.01 g), be placed in 50mL tool screw lid polypropylene centrifuge tube, add standard liquid, 1.5 g trichloroacetic acids, after vortex mixing 30 s, centrifugal 10 min under 4 ℃, 14000 r/min.Collect supernatant in another 50mL centrifuge tube, and transfer pH to 7.0 with sodium hydroxide solution, screw screw lid, vortex mixing 30 s, centrifugal 10 min under 4 ℃, 14000 r/min again, draw clear liquid and be settled to 15mL in another 50mL centrifuge tube and water, then transfer them in the flat sample bottle that 20mL is placed with miniature stirrer, wait to extract.
Hollow fiber conduit is immersed ultrasonic 10 min in n-octyl alcohol/toluene solution, make in the hole on the doughnut tube wall to be full of organic solvent.With micro syringe with the solvent sucking-off in the doughnut tube chamber, only make fiber tube wall and micropore be full of solvent, then draw n-octyl alcohol/toluene solution (v:v=1:1) of 50 μ L with syringe, syringe needle is inserted its inner chamber from hollow fiber conduit one end, the pushing syringe piston, organic solvent is pushed in the inner chamber of hollow fiber conduit, and port is sealed.Hollow fiber conduit one end is fixed on silica gel piece, the hollow fiber conduit that solvent is housed all is immersed in in phase solution, again with sample bottle as in micro-wave oven, microwave 10 s under the 400W microwave power, taking-up is placed on magnetic stirring apparatus, 500 r/min stir 3 min, repetitive operation four times, extraction time 12.67 min: collect the interior remaining whole solvents of hollow fiber conduit to interpolation pipe, and dry up in the nitrogen concentrating instrument, use at last the methanol/water solution of (v:v=1:4) to be settled to 100 μ L, measure for LC-MS/MS.
Claims (7)
1. a microwave is assisted-doughnut-liquid/liquid micro-extraction device, it is characterized in that it comprises: doughnut tube material, organic solvent, silica gel piece, magnetic stir bar, magnetic stirring apparatus and micro-wave oven.
Microwave according to claim 1 auxiliary-preparation method of doughnut-liquid/liquid micro-extraction device, comprise the following steps: (1) is cleaned hollow fiber conduit to dry and with sealing machine, an end is wherein sealed afterwards, (2) a certain amount of organic solvent is injected in hollow fiber conduit, (3) will be fixed on silica gel piece after other end sealing, (4) are placed in sample flasket with hollow fiber conduit and are prepared into micro-extraction device again.
According to claim 1-2 described microwaves auxiliary-doughnut-liquid/liquid micro-extraction device, the material that it is characterized in that doughnut can be all have pore diameter range at nanoscale to micron-sized microporous hollow fiber pipe.
4. according to claim 1-2 described microwaves are assisted-doughnut-liquid/liquid micro-extraction device, it is characterized in that organic solvent and hollow fiber conduit have stronger affinity.
According to claim 1-4 described microwaves auxiliary-doughnut-liquid/liquid micro-extraction device, it is characterized in that described organic solvent and target compound to be analyzed have preferably dissolubility, suitable viscosity is arranged, volatility is low and polarity is less.
6. according to claim 1-2 described microwaves are assisted-doughnut-liquid/liquid micro-extraction device, it is characterized in that micro-wave oven can be all household microwave oven or professional microwave synthesis devices with 915 megahertzes or 2450 megahertzes.
7. according to claim 1-4 described microwaves are assisted-doughnut-liquid/liquid micro-extraction device, it is characterized in that being applied to extraction, purification, separation and the enrichment of sample pre-treatments.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103293042A (en) * | 2013-06-17 | 2013-09-11 | 山西医科大学 | Method and device for micro-extracting filter membrane headspace solvent |
| CN104165793A (en) * | 2014-08-29 | 2014-11-26 | 深圳出入境检验检疫局食品检验检疫技术中心 | Microwave-assisted-hollow fiber-liquid/solid extraction device and microextraction method |
| CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
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| US20070113616A1 (en) * | 2003-12-09 | 2007-05-24 | Beat Schilling | Device for sample preparation |
| CN102620968A (en) * | 2012-04-09 | 2012-08-01 | 红河学院 | Detection method for organic pesticide residue sample by pretreatment of support ionic liquid film |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070113616A1 (en) * | 2003-12-09 | 2007-05-24 | Beat Schilling | Device for sample preparation |
| CN102620968A (en) * | 2012-04-09 | 2012-08-01 | 红河学院 | Detection method for organic pesticide residue sample by pretreatment of support ionic liquid film |
Non-Patent Citations (2)
| Title |
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| CHANBASHA BASHEER: "Analysis of persistent organic pollutants in marine sediments using a novel microwave assisted solvent extraction and liquid-phase microextraction technique", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 付华峰: "中空纤维膜液相微萃取-HPLC法测定复方穿心莲片中脱水穿心莲内酯含量", 《药物分析杂志》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103293042A (en) * | 2013-06-17 | 2013-09-11 | 山西医科大学 | Method and device for micro-extracting filter membrane headspace solvent |
| CN103293042B (en) * | 2013-06-17 | 2016-01-20 | 山西医科大学 | Filter membrane head space solvent extraction method and device |
| CN104165793A (en) * | 2014-08-29 | 2014-11-26 | 深圳出入境检验检疫局食品检验检疫技术中心 | Microwave-assisted-hollow fiber-liquid/solid extraction device and microextraction method |
| CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
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Inventor after: Zhang Yi Inventor after: Yue Zhenfeng Inventor after: Chen Peijin Inventor after: Xiao Feng Inventor after: Lin Li Inventor after: Liang Tongwen Inventor after: Lin Shanshan Inventor before: Zhang Yi Inventor before: Lin Shanshan Inventor before: Yue Zhenfeng Inventor before: Zheng Zongkun Inventor before: Zhao Fengjuan |
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