CN102313665A - Liquid-liquid micro extraction method for ultrasonic atomized and strengthened suspension drop type ion liquid - Google Patents

Liquid-liquid micro extraction method for ultrasonic atomized and strengthened suspension drop type ion liquid Download PDF

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CN102313665A
CN102313665A CN2010102159917A CN201010215991A CN102313665A CN 102313665 A CN102313665 A CN 102313665A CN 2010102159917 A CN2010102159917 A CN 2010102159917A CN 201010215991 A CN201010215991 A CN 201010215991A CN 102313665 A CN102313665 A CN 102313665A
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liquid
micro
ionic liquid
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蔡美强
金米聪
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Zhejiang Gongshang University
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Zhejiang Gongshang University
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Abstract

The invention discloses a liquid-liquid micro extraction method for ultrasonic atomized and strengthened suspension drop type ion liquid, which comprises the following steps that: 1) an ultrasonic transducer is arranged at the bottom of an extraction container, liquid and a sample bottle are arranged in the extraction container, liquid sample to be analyzed is arranged in the sample bottle, and a micro injector is hanged in the sample bottle and on the liquid sample to be analyzed; 2) ion liquid is sucked by the micro injector so as to be hanged at a needle opening to form suspended ion liquid drops; 3) the ultrasonic transducer is started to atomize the liquid sample to be analyzed, and then timing is started; and 4) when the set time of 360-1000 seconds is up for the ultrasonic transducer 2, the ultrasonic transducer is turned off, the ion liquid is sucked into the micro injector, and the concentration of the liquid sample to be analyzed is detected by an analytic instrument. The invention has the advantages that the operation is simple, the interference of impurities can be reduced, the rate of enrichment is higher, the reproducibility is good, the recovery rate is high, the promotion can be facilitated, and the method can be applied in detection of organic substances of food samples, environments, organisms and other complex matrixes and has broad application prospects.

Description

Ultrasonic atomizatio is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method
Technical field
The present invention relates to separating substances and analysis technical field, relate in particular to a kind of ultrasonic atomizatio and strengthen hanging drop type ionic liquid liquid-liquid micro-extraction method.
Background technology
Environment is a comprehensive and complicated system, and environmental sample varies, because its complicacy and singularity make specimen preparation and pretreatment technology in Environmental Analytical Chemistry, occupy special status.Required time of sample pre-treatments is the longest, accounts for 2/3rds of whole sample analytic process, and its success or not is directly connected to the analysis speed of sample and the degree of accuracy and the reappearance of whole mensuration.Yet along with the develop rapidly of modern analysis determining instrument, the sample pre-treatments technology does not but obtain enough attention, and the research of sample preparation methods relatively lags behind, and becomes the bottleneck of present analytical chemistry.Relating to all fundamental research fields such as medicine, environmental protection, life science, petrochemical complex; Often demand side is to various matrix are complicated, tested component concentration is extremely low sample; Therefore, sample carried out assay determination before, it is carried out suitable pre-treatment is very important.Up to now, nearly tens kinds of various sample-pretreating methods, that uses morely also has tens kinds.Yet these traditional sample-pretreating methods exist that labour intensity is big, the time cycle is long, need use in a large number the disagreeableness poisonous organic solvent of environment sometimes, be difficult to realize wretched insufficiency such as robotization.Therefore, the R and D of sample-pretreating method and technology have caused the concern of vast AC, and the exploration of various new technologies and new method and research have become the advanced subject of contemporary analytical chemistry.Easy and simple to handle, quick, reagent dosage few (or without reagent), microminiaturization, robotization or semi-automation, the method for separating and concentrating that is easy to combine with various detection meanss become a research direction of current environment analysis field, and various micro-extraction techniques arise at the historic moment.The SPME method
SPME method (Solid phase microextraction; SPME) be the new extraction and separation technology that on the basis of SPE, grows up; Use the SPME extracting head that the analyte in the sample is extracted, and then utilize the high temperature of gas chromatography injection port or the moving phase of high performance liquid chromatography or the buffer solution of Capillary Electrophoresis etc. that the analyte that extracts is carried out desorb.The SPME method has been widely used in the analysis of organic contaminant in the various complex samples.Desorption rate is slow, is prone to cause the chromatographic peak hangover of analyte.When SPME and high performance liquid chromatography coupling; Need a special desorption apparatus, and analyte desorption needs considerable time fully, because there are competitive Adsorption in sample substrate and coating to determinand in the extraction process; So coating is very important to the size of analyte affinity.The extracting head of the extensive stockization that SPME is used, selectivity is strong, but broken easily in the operating process, has strengthened analysis cost.
Liquid-phase micro-extraction
Liquid-phase micro-extraction method (LPME) is a kind of new sample-pretreating method that on liquid-liquid extraction (LLE) and SPME (SPME) basis, grows up; Its centralized procurement appearance, extract, concentrate in one; Inner through 1 organic solvent being suspended from chromatogram sample introduction syringe needle or organic solvent being injected a bit of hollow fiber, and place solution to be measured (directly immersed method) or on (head space method) separation and concentration test substance.LPME and SPME are all simple, convenient, but the LPME cost is low more than SPME, thereby receive publicity.
Ionic liquid has that steam forces down, Heat stability is good, solubility property are high, can establish characteristics such as juice property and diversity, makes it developed rapidly and use aspect micro-extraction extracting especially.And in single micro-extraction, dispersion liquid phase extraction, liquid-liquid one liquid micro-extraction and SPME; Ionic liquid is more with its bigger viscosity, density and characteristic such as non-volatile; Make micro-extraction technique operate more easily; Organic solvent pollution, the sensitivity of method is higher, and has expanded the range of application of micro-extraction.It is few that the ionic liquid micro-extraction has a consumption, the high characteristics of accumulation rate, but be suitable for the high organism of volatility.Single micro-extraction ionic liquid drips the benzene series thing (like benzene, toluene, ethylbenzene, o-xylene, m-xylene, P-xylene) that application aspect the micro-extraction concentrates on the extract and separate environment mostly at the head space list.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, provide a kind of ultrasonic atomizatio to strengthen hanging drop type ionic liquid liquid-liquid micro-extraction method.
Ultrasonic atomizatio is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method and is comprised the steps:
1) in the extraction container bottom ultrasonic transducer is installed, is provided with liquid and sample bottle in the extraction container, in sample bottle, be placed with fluid sample to be analyzed, with fluid sample overhung to be analyzed micro syringe is arranged in the sample bottle;
2) micro syringe is drawn ionic liquid and is made it to be suspended on the pin mouth, forms the ionic liquid hanging drop;
3) the startup ultrasonic transducer makes fluid sample atomizing to be analyzed and picks up counting;
4) after ultrasonic transducer 2 reaches 360~1000 seconds setting-up times, close ultrasonic transducer, ionic liquid is inhaled back micro syringe, detect fluid sample concentration to be analyzed with analytical instrument.
Described ionic liquid is disubstituted imidazole class ionic liquid or tri-substituted imidazole class ionic liquid; Described ultrasonic transducer 2 frequencies are 70KHZ~1MHZ, and power is 100~200W; Described sample bottle is one or more.Described fluid sample to be analyzed is drinox, dieldrite, endrin, Niran, heptachlor, DDT, mirex, toxaphene, hexachloro-benzene, polychlorinated biphenyl, PCDD or PCDF.The volume of described ionic liquid hanging drop is 1~4 μ L.Described analytical instrument is chromatograph or chromatography-mass spectroscopy appearance.
The sample requirement that the present invention proposes ultrasonic atomizatio reinforcement hanging drop type ionic liquid liquid-liquid micro-extraction method is few; Only consume the organic solvent of micro updating; Can get rid of the interference of coexistence component in the complex matrices such as food, environment and biology; Reduce analysis cost, very convenient with the coupling of liquid chromatography, gas chromatography, liquid chromatography-mass spectrography (tandem mass spectrum) and gas chromatography-mass spectrum analytical approachs such as (tandem mass spectrums).Compare with the liquid-phase microextraction method of reporting for work, have easy and simple to handle, process stabilization and various article and extract simultaneously, can improve sample pre-treatments speed and degree of accuracy.
Description of drawings
Fig. 1 is that ultrasonic atomizatio is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction apparatus structure synoptic diagram; Among the figure: micro syringe is quantitative 1, ultrasonic transducer 2, ionic liquid 3, extraction container 4, sample bottle 5;
Fig. 2 is in the seawater 2, and the 3-DCBP is measured chromatogram;
Fig. 3 is a variable concentrations 2,3-DCBP enrichment figure;
Fig. 4 is variable concentrations mirex enrichment figure;
Fig. 5 is variable concentrations hexachloro-benzene enrichment figure;
Fig. 6 is variable concentrations toxaphene enrichment figure.
Embodiment
Principle of the present invention is: ultrasound wave has undulatory property, high frequency characteristics and thermal characteristics or non-thermal characteristics characteristics such as (biological effects).The present invention utilizes hyperacoustic thermal effect and mechanical effect can strengthen organism volatilization extraction efficiency; Promptly utilize ultrasonic heating to quicken organism volatilization, enhance liquid sample volatilization area, improve organic speed of ionic liquid enrichment and efficient, obtained higher enrichment multiple (.Also liquid is to the extraction process of target extract in the fluid sample (mainly being organic compound).The ultrasonic atomization system can be divided into two big types according to the type of atomization tank: hermetic type microwave atomizing system with open pot type atomizing system; According to the characteristics of micro-extraction, ultrasound wave acts on extraction system (sample) and adopts hermetic type microwave atomizing system in this method.
Ultrasonic atomizatio is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method and is comprised the steps:
1) ultrasonic transducer 2 is installed in extraction container 4 bottoms, is provided with liquid and sample bottle 5 in the extraction container 4, in sample bottle 5, be placed with fluid sample to be analyzed, with fluid sample overhung to be analyzed micro syringe 1 is arranged in the sample bottle 5;
2) micro syringe 1 is drawn ionic liquid and is made it to be suspended on the pin mouth, forms the ionic liquid hanging drop;
3) startup ultrasonic transducer 2 makes fluid sample atomizing to be analyzed and picks up counting;
4) after ultrasonic transducer 2 reaches 360~1000 seconds setting-up times, close ultrasonic transducer 2, ionic liquid 3 is inhaled back micro syringe 1, detect fluid sample concentration to be analyzed with analytical instrument.
Described ionic liquid is disubstituted imidazole class ionic liquid or tri-substituted imidazole class ionic liquid; Described ultrasonic transducer 2 frequencies are 70KHZ~1MHZ, and power is 100~200W; Described sample bottle 5 is one or more.Described fluid sample to be analyzed is drinox, dieldrite, endrin, Niran, heptachlor, DDT, mirex, toxaphene, hexachloro-benzene, polychlorinated biphenyl, PCDD or PCDF.The volume of described ionic liquid hanging drop is 1~4 μ L.Described analytical instrument is chromatograph or chromatography-mass spectroscopy appearance.
Embodiment 1:
Strengthen polychlorinated biphenyl in the suspension type ionic liquid liquid-liquid micro-extraction seawater with ultrasonic atomizatio, step is following: get the seawater 10mL that receives pollution by polychlorinated biphenyles and place in the sample bottle; Sample bottle is put into the extraction container that fills water, and the setting ultrasonic frequency is 600KHZ, and power is 200W; Micro syringe is drawn ionic liquid 1-butyl one 3 monomethyl imidazoles hexafluorophosphates 1 μ L, and is it is disposable, quantitatively hang on micro syringe; Start ultrasonic transducer, pick up counting; When timing reaches 360s, close ultrasonic transducer, ionic liquid is inhaled back micro syringe; In gas chromatograph, carry out the gas chromatographic analysis of hanging drop type thermal desorption.Fig. 3 is the chromatogram that obtains, and strengthens suspension type ionic liquid liquid-liquid micro-extraction through ultrasonic atomizatio, and target organism polychlorinated biphenyl has obtained enrichment effectively and purifying, has reduced the unit number and the burden of subsequent analysis process.
Embodiment 2:
In the seawater 2; The 3-DCBP is a 500ng/L methanol-water solution; Get 0.1,0.2,0.3,0.4 respectively, 0.5mL places the 100mL volumetric flask, adds deionized water and is diluted to scale, makes sample; Sample liquids is carried out ultrasonic atomizatio strengthen suspension type ionic liquid liquid-liquid micro-extraction, step is following: get the seawater 10mL that receives pollution by polychlorinated biphenyles and place in the sample bottle; Sample bottle is put into the extraction container that fills water, and the setting ultrasonic frequency is 600KHZ, and power is 100W; Micro syringe is drawn ionic liquid 1 μ L, and is it is disposable, quantitatively hang on the micro syringe syringe needle; Start ultrasonic transducer, pick up counting; When timing reaches 450s, close ultrasonic transducer, ionic liquid is inhaled back micro syringe; On gas chromatograph, carry out the gas chromatographic analysis of hanging drop type thermal desorption, obtain 2, the concentration of 3-DCBP.Initial concentration and the corresponding figure of being of the concentration that records with surveying water sample obtain Fig. 3. and can see that both linearly dependent coefficients are 0.997, the concentration of extraction phase reaches 2,28 times of 3-DCBP.Explain that ultrasonic atomizatio reinforcement suspension type ionic liquid liquid-liquid micro-extraction and gas phase coupling are fit to the quantitative test of trace organic substance in the environmental water sample; The concentration effect that ultrasonic atomizatio is strengthened suspension type ionic liquid liquid-liquid micro-extraction makes chromatogram to 2, and the detectability of 3-DCBP has descended more than 10 times.
Embodiment 3:
Compound concentration is the mirex methanol-water solution of 0.5mg/L; Get 1,2,3,4 respectively, 5mL places the 100mL volumetric flask; Add deionized water and be diluted to scale; Make sample, sample liquids is carried out ultrasonic atomizatio strengthen suspension type ionic liquid liquid-liquid micro-extraction, step is following: sample thief 20mL places in the sample bottle; Sample bottle is put into the extraction container that fills water, and the setting ultrasonic frequency is 1MHZ, and power is 200W; Micro syringe is drawn 1-butyl-3-methylimidazole fluoroform sulphonate 2 μ L, and is it is disposable, quantitatively hang on the micro syringe syringe needle; Start ultrasonic transducer, pick up counting; When timing reaches 600s, close ultrasonic transducer, ionic liquid is inhaled back micro syringe; Carry out liquid-phase chromatographic analysis, obtain the concentration of mirex.Initial concentration and the corresponding figure of being of the concentration that records with surveying water sample obtain Fig. 4.
Embodiment 4:
Compound concentration is the WS hexachloro-benzene methanol-water solution of 0.8mg/L; Get 1,2,3 respectively, 4mL places the 100mL volumetric flask; Add deionized water and be diluted to scale; Make sample, sample liquids is carried out ultrasonic atomizatio strengthen suspension type ionic liquid liquid-liquid micro-extraction, step is following: sample thief 5mL places in the sample bottle; Extraction flask is put into the extraction container that fills water, and the setting ultrasonic frequency is 800KHZ, and power is 200W; Micro syringe is drawn 1-ethyl-3-methyl imidazolium tetrafluoroborate 2 μ L, and is it is disposable, quantitatively hang on the micro syringe syringe needle; Start ultrasonic transducer, pick up counting; When timing reaches 800s, close ultrasonic transducer, ionic liquid is inhaled back micro syringe; Carry out the gas chromatographic analysis of hanging drop type thermal desorption, obtain the concentration of hexachloro-benzene.Initial concentration and the corresponding figure of being of the concentration that records with surveying water sample obtain Fig. 5.
Embodiment 5:
Compound concentration is the WS toxaphene methanol-water solution of 0.6mg/L; Get 1,2,3 respectively, 4mL places the 100mL volumetric flask; Add deionized water and be diluted to scale; Make sample, sample liquids is carried out ultrasonic atomizatio strengthen suspension type ionic liquid liquid-liquid micro-extraction, step is following: sample thief 2mL places in the sample bottle; Sample bottle is put into the extraction container that fills water, and the setting ultrasonic frequency is 800KHZ, and power is 200W; Micro syringe is drawn the two fluoroform sulfimide salt 1 μ L of 1-butyl-3-methylimidazole, and is it is disposable, quantitatively hang on syringe needle; Start ultrasonic transducer, pick up counting; When timing reaches 1000s, close ultrasonic transducer, ionic liquid is inhaled back micro syringe; Carry out the gas chromatographic analysis of hanging drop type thermal desorption, obtain the concentration of toxaphene.Initial concentration and the corresponding figure of being of the concentration that records with surveying water sample obtain Fig. 6. can see that both linearly dependent coefficients are good.

Claims (7)

1. a ultrasonic atomizatio is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method, it is characterized in that comprising the steps:
1) in extraction container (4) bottom ultrasonic transducer (2) is installed; Be provided with liquid and sample bottle (5) in the extraction container (4); In sample bottle (5), be placed with fluid sample to be analyzed, with fluid sample overhung to be analyzed micro syringe (1) arranged in the sample bottle (5);
2) micro syringe (1) is drawn ionic liquid and is made it to be suspended on the pin mouth, forms the ionic liquid hanging drop;
3) startup ultrasonic transducer (2) makes fluid sample atomizing to be analyzed and picks up counting;
4) ultrasonic transducer (2) reaches 360~1000 seconds and cuts out ultrasonic transducer (2) behind the setting-up time, and ionic liquid (3) is inhaled back micro syringe (1), detects fluid sample concentration to be analyzed with analytical instrument.
2. a kind of ultrasonic atomizatio according to claim 1 is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method, it is characterized in that described ionic liquid is disubstituted imidazole class ionic liquid or tri-substituted imidazole class ionic liquid.
3. a kind of ultrasonic atomizatio according to claim 1 is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method, it is characterized in that described ultrasonic transducer (2) frequency is 70KHZ~1MHZ, and power is 100~200W.
4. a kind of ultrasonic atomizatio according to claim 1 is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method, it is characterized in that described sample bottle 5 is one or more.
5. a kind of ultrasonic atomizatio according to claim 1 is strengthened hanging drop type ionic liquid liquid-liquid micro-extraction method, it is characterized in that described fluid sample to be analyzed is drinox, dieldrite, endrin, Niran, heptachlor, DDT, mirex, toxaphene, hexachloro-benzene, polychlorinated biphenyl, PCDD or PCDF.
6. strengthen hanging drop type ionic liquid liquid-liquid micro-extraction method according to the described a kind of ultrasonic atomizatio of claim, the volume that it is characterized in that described ionic liquid hanging drop is 1~4 μ L.
7. strengthen hanging drop type ionic liquid liquid-liquid micro-extraction method according to the described a kind of ultrasonic atomizatio of claim, it is characterized in that described analytical instrument is chromatograph or chromatography-mass spectroscopy appearance.
CN2010102159917A 2010-06-30 2010-06-30 Liquid-liquid micro extraction method for ultrasonic atomized and strengthened suspension drop type ion liquid Pending CN102313665A (en)

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Application publication date: 20120111