CN104162416A - Polyether sulfone ketone coating solid phase micro extraction bar and preparation method thereof - Google Patents
Polyether sulfone ketone coating solid phase micro extraction bar and preparation method thereof Download PDFInfo
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- CN104162416A CN104162416A CN201410407905.0A CN201410407905A CN104162416A CN 104162416 A CN104162416 A CN 104162416A CN 201410407905 A CN201410407905 A CN 201410407905A CN 104162416 A CN104162416 A CN 104162416A
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Abstract
The invention relates to a polyether sulfone ketone coating solid phase micro extraction bar and a preparation method thereof. The method comprises the following steps: adding solid-state polyether sulfone ketone into a solvent, stirring until the polyether sulfone ketone is completely dissolved, standing in a dry environment, thus obtaining polyether sulfone ketone solution; by taking a magnetic rotor as a carrier of the solid phase micro extraction bar, immersing the cleaned magnetic rotor into the polyether sulfone ketone solution, taking out the rotor, immediately putting the magnetic rotor into a coagulating bath, soaking for 0.5-30 minutes, taking out the magnetic rotor and putting into deionized water, soaking for 24-72 hours, taking out the magnetic rotor and drying at normal temperature; preserving the temperature of the dried magnetic rotor to the temperature of 40-100 DEG C for 0.1-1 hour under inert gas shielding; raising the temperature to 100-180 DEG C, and preserving the temperature for 1-6 hours; and finally, raising the temperature to 240-290 DEG C, aging for 1-6 hours, thus obtaining the polyether sulfone ketone coating solid phase micro extraction bar. With the adoption of the extraction bar prepared by the invention, the extraction ratio can be improved, and the extraction bar has high extraction capacity on trace polar semi-volatile and volatile substances.
Description
Technical field
The present invention relates to a kind of Sample Pretreatment Technique in analytical chemistry field, particularly relate to a kind of preparation method of polyethersulfone ketone coating solid phase micro-extraction rod, and the polyethersulfone ketone coating solid phase micro-extraction rod of preparing by the method.
Background technology
Traditional Sample Pretreatment Technique mostly needs to use a large amount of organic solvents, not only contaminated environment but also serious harm worker's health of human body, and complex operation, time and effort consuming, poor reproducibility.SPME (English abbreviation SPME) is the Sample Pretreatment Technique of early 1990s development.Because it is simple to operate, sample requirement is little, without extractant, high repeatability and other advantages, since coming out, it is subject to researcher's extensive concern.Although SPME technology has above plurality of advantages, because its fiber material is coated on quartz fibre, the volume of fixing phase has had a strong impact on the rate of recovery and the sensitivity measured.Under growing low detectability and highly sensitive demand, SPME technology can not meet the requirement of analyzing and testing completely.In order to address this problem, the people such as Belgian Sandra in 1999 have been developed solid-state stirring rod abstraction technique (English abbreviation SBSE).This technology has replaced the quartz fibre in SPME technology by absorption stirring rod, applies or puts sorbing material on the surface of stirring rod, therefore extracts stationary phase volume than the large 50-500 of SPME doubly, and adsorption surface area is large, the corresponding raising of enrichment times.While extraction, adsorb stirring rod self simultaneously and complete stirring, avoided the competitive Adsorption of stirrer in SPME technology, therefore this technology is very suitable for the enrichment of trace organic component in sample.The extraction coating of extraction bar mostly adopts dimethyl silicone polymer (English abbreviation PDMS) at present, this coating material is relatively suitable for extracting the compound of low pole, and poor for the effect of extracting of stronger polar organic matter, limit the range of application of this technology.For this puzzlement, researcher has also developed the coating material of numerous applicable extraction polar compounds.Wherein, the most noticeable the is high diazanaphthalene terphenyl polyethersulfone ketone (PPESK) that waits people's exploitation of the not smoothgoing tin of Dalian University of Technology, it has high temperature resistant, strong alkali-acid resistance, organic solvent-resistant, mechanical strength high; Sulfuryl, carbonyl and π in polyethersulfone ketone molecular structure-pi-conjugated polar functional group, very easily with polar group generation conjugation.The people such as the sight Wen Na of Dalian Chemical Physics Research Institute first by PPESK for the preparation of SPME pin, extraction polar compound obtained good effect.Mentioned above, the enrichment times of SBSE than the high decades of times of SPME to hundreds of times, if by PPESK for the preparation of SPME rod, will expand greatly the range of application of SBSE technology.Therefore the present invention adopts a kind of polyethersulfone ketone coating to prepare SPME rod, and develop the preparation method that PPESK solid phase is extraction bar.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of polyethersulfone ketone coating solid phase micro-extraction rod, and the polyethersulfone ketone coating solid phase micro-extraction rod of preparing by the method.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of polyethersulfone ketone coating solid phase micro-extraction rod, and it comprises:
Step 1, joins solid-state polyethersulfone ketone in solvent and is stirred to completely and dissolves, and in dry environment, leaves standstill, and obtains polyethersulfone ketone solution;
Step 2, a kind of in dimethylacetylamide (DMAc), 1-METHYLPYRROLIDONE (NMP), dimethyl formamide (DMF) and dimethyl sulfoxide (DMSO) (DMSO) or their mixture are mixed with deionized water, obtain coagulating bath;
Step 3, the carrier using magnet rotor as SPME rod, immerses polyethersulfone ketone solution by clean magnet rotor, after taking-up, put into immediately coagulating bath, soak 0.5～30 minute, after taking-up, put into deionized water, soak 24～72 hours, then take out and be dried at normal temperatures;
Step 4, dried magnet rotor 40～100 DEG C of constant temperature 0.1～1 hour under inert gas shielding; Then be warmed up to 100～180 DEG C, constant temperature 1～6 hour; Finally be warmed up to 240～290 DEG C, aging 1～6 hour, make polyethersulfone ketone coating solid phase micro-extraction rod.
The preparation method of polyethersulfone ketone coating solid phase micro-extraction rod as above, solvent described in step 1 is a kind of in dimethylacetylamide (DMAc), 1-METHYLPYRROLIDONE (NMP), dimethyl formamide (DMF) and dimethyl sulfoxide (DMSO) (DMSO) or their mixture.In step 1, the weight proportion of polyethersulfone ketone and solvent is 1:3～9.
The invention has the beneficial effects as follows: 1, improve extraction multiple, trace polarity half volatile/volatile materials is had to higher extracting power.2, applied range, can expand the range of application of pre-treatment.3, economical and practical, cost is low, reusable.4, operating efficiency is high, easy operating, convenient and swift.
The present invention also provides a kind of use polyethersulfone ketone coating solid phase micro-extraction rod that as above prepared by any one method.
Brief description of the drawings
Fig. 1 is the gas chromatogram of extraction Trace Phenols in Water class material.
Fig. 2 is the gas chromatogram of trace nitrobenzene substances in extraction water.
Detailed description of the invention
Below in conjunction with accompanying drawing, principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Magnet rotor used in following examples is prepared by the following method: the material of magnet rotor is iron core and glass tube.Its preparation process is as follows: first, by certain specification cutting glass tube, and will manage an end closure on flame.Then, intercept certain length iron core, put into the glass tube of an end closure, and adopt to use the same method the other end is sealed.
Embodiment 1
Step 1, joins solid-state 2.0g polyethersulfone ketone in 10.0g dimethylacetylamide and is stirred to completely and dissolves, and leaves standstill 48h in dry environment, obtains polyethersulfone ketone solution;
Step 2, mixes with deionized water dimethylacetylamide by the volume ratio of 1:1, obtain coagulating bath;
Step 3, the carrier using magnet rotor as SPME rod, immerses polyethersulfone ketone solution by clean magnet rotor, after taking-up, put into immediately coagulating bath, soak 30 minutes, after taking-up, put into deionized water, soak 36 hours, then take out and be dried at normal temperatures;
Step 4, by dried magnet rotor 50 DEG C of constant temperature 1 hour under helium protection; Then be warmed up to 180 DEG C, constant temperature 6 hours; Finally be warmed up to 240 DEG C, aging 2 hours, make the polyethersulfone ketone coating solid phase micro-extraction rod of embodiment 1.
Embodiment 2
Step 1, joins solid-state 2.0g polyethersulfone ketone in 6.0g 1-METHYLPYRROLIDONE and is stirred to completely and dissolves, and leaves standstill 32h in dry environment, obtains polyethersulfone ketone solution;
Step 2, mixes with deionized water 1-METHYLPYRROLIDONE by the volume ratio of 1:1, obtain coagulating bath;
Step 3, the carrier using magnet rotor as SPME rod, immerses polyethersulfone ketone solution by clean magnet rotor, after taking-up, put into immediately coagulating bath, soak 30 minutes, after taking-up, put into deionized water, soak 24 hours, then take out and be dried at normal temperatures;
Step 4, by dried magnet rotor 40 DEG C of constant temperature 0.5 hour under helium protection; Then be warmed up to 120 DEG C, constant temperature 5 hours; Finally be warmed up to 290 DEG C, aging 4 hours, make the polyethersulfone ketone coating solid phase micro-extraction rod of embodiment 2.
Embodiment 3
Step 1, joins solid-state 2.0g polyethersulfone ketone in 8.0g dimethyl formamide and is stirred to completely and dissolves, and leaves standstill 50h in dry environment, obtains polyethersulfone ketone solution;
Step 2, mixes with deionized water dimethyl formamide by the volume ratio of 1:1, obtain coagulating bath;
Step 3, the carrier using magnet rotor as SPME rod, immerses polyethersulfone ketone solution by clean magnet rotor, after taking-up, put into immediately coagulating bath, soak 10 minutes, after taking-up, put into deionized water, soak 72 hours, then take out and be dried at normal temperatures;
Step 4, by dried magnet rotor 100 DEG C of constant temperature 1 hour under neon gas protection; Then be warmed up to 100 DEG C, constant temperature 4 hours; Finally be warmed up to 260 DEG C, aging 6 hours, make the polyethersulfone ketone coating solid phase micro-extraction rod of embodiment 3.
Application examples 1
Utilize the aldehydes matter that adopts embodiment 1 gained extraction bar extraction underwater trace, by thermal desorption device, aldehydes matter is transferred to (GC 7890A Agilent) in gas-chromatography again, utilize the retention time difference of each material in chromatographic column, be isolated.Gained gas chromatogram is Fig. 1.Sample concentration: 5ng/mL; Sample volume: 20mL; Extraction temperature: 40 DEG C; Extraction time: 20min; Salinity: 10%; Mixing speed: 760rpm.
Gas chromatograph condition: chromatographic column: SE-54,30m × 320um × 0.4um; Post flow: 2ml/min.
Wherein the aldehydes matter of underwater trace is: 1,2-chlorophenol (2-Chlorophenol); 2,2-sylvan (2-Methylphenol); 3,2-nitrophenols (2-Nitrophenol); 4,2,4-Dichlorophenol (2,4-Dichlorophenol); 5,2,4,6-trichlorophenol (2,4,6-Trichlorophenol).
Application examples 2
Utilize the nitrobenzene matters of embodiment 2 gained extraction bar extraction underwater traces, by thermal desorption device, nitrobenzene matters is transferred to (GC 7890A Agilent) in gas-chromatography again, utilize the retention time difference of each material in chromatographic column, be isolated.Gained gas chromatogram is Fig. 2.Sample concentration: 2ng/mL; Sample volume: 20mL; Extraction temperature: 50 DEG C; Extraction time: 30min; Salinity: 30%; Mixing speed: 800rpm.
Gas chromatograph condition: chromatographic column: SE-54,30m × 320um × 0.4um; Post flow: 2ml/min.
Wherein the nitrobenzene matters of underwater trace is: 1, and nitrobenzene (Nitrobenzene); 2,2-nitrotoleune (2-Nitrotoluene); 3,4-nitrotoleune (4-Nitrotoluene); 4,2,4-dinitrotoluene (DNT) (2,4-Dinitrotoluene).
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a preparation method for polyethersulfone ketone coating solid phase micro-extraction rod, its spy is, comprising:
Step 1, joins solid-state polyethersulfone ketone in solvent and is stirred to completely and dissolves, and in dry environment, leaves standstill, and obtains polyethersulfone ketone solution;
Step 2, mixes a kind of in dimethylacetylamide, 1-METHYLPYRROLIDONE, dimethyl formamide and dimethyl sulfoxide (DMSO) or their mixture with deionized water, obtain coagulating bath;
Step 3, the carrier using magnet rotor as SPME rod, immerses polyethersulfone ketone solution by clean magnet rotor, after taking-up, put into immediately coagulating bath, soak 0.5～30 minute, after taking-up, put into deionized water, soak 24～72 hours, then take out and be dried at normal temperatures;
Step 4, by dried magnet rotor 40～100 DEG C of constant temperature 0.1～1 hour under inert gas shielding; Then be warmed up to 100～180 DEG C, constant temperature 1～6 hour; Finally be warmed up to 240～290 DEG C, aging 1～6 hour, make polyethersulfone ketone coating solid phase micro-extraction rod.
2. the preparation method of polyethersulfone ketone coating solid phase micro-extraction rod according to claim 1, it is characterized in that, solvent described in step 1 is a kind of in dimethylacetylamide, 1-METHYLPYRROLIDONE, dimethyl formamide and dimethyl sulfoxide (DMSO) or their mixture.
3. the preparation method of polyethersulfone ketone coating solid phase micro-extraction rod according to claim 1, is characterized in that, in step 1, the weight proportion of polyethersulfone ketone and solvent is 1:3～9.
4. the preparation method of polyethersulfone ketone coating solid phase micro-extraction rod according to claim 1, is characterized in that, in step 2, coagulating bath is the mixed solution of deionized water and one or more solvents, and the volume ratio of deionized water and solvent is 0.1～10.
5. the preparation method of polyethersulfone ketone coating solid phase micro-extraction rod according to claim 1, it is characterized in that, step 3, carrier using magnet rotor as SPME rod, immerses polyethersulfone ketone solution by clean magnet rotor, puts into immediately coagulating bath after taking-up, soak 0.5～30 minute, after taking-up, put into deionized water, soak 24～72 hours, then take out and be dried at normal temperatures.
6. a polyethersulfone ketone coating solid phase micro-extraction rod of preparing by the method for claim 1-5 any one.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11565193B2 (en) * | 2017-04-11 | 2023-01-31 | Shimadzu Corporation | Component extraction apparatus |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143272A (en) * | 2006-09-15 | 2008-03-19 | 中国科学院大连化学物理研究所 | Method for preparing poly (phthalazinone ether sulfone ketone) solid phase micro-extracting fiber head |
| WO2013068026A1 (en) * | 2011-11-07 | 2013-05-16 | Tehran University Of Medical Sciences (Tums), Faculty Of Environmental University Of Tehran | Development of a new coating for sorptive extraction by stir bars |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101143272A (en) * | 2006-09-15 | 2008-03-19 | 中国科学院大连化学物理研究所 | Method for preparing poly (phthalazinone ether sulfone ketone) solid phase micro-extracting fiber head |
| WO2013068026A1 (en) * | 2011-11-07 | 2013-05-16 | Tehran University Of Medical Sciences (Tums), Faculty Of Environmental University Of Tehran | Development of a new coating for sorptive extraction by stir bars |
Non-Patent Citations (2)
| Title |
|---|
| JOURNAL OF CHROMATOGRAPHY A: ""Poly(phthalazine ether sulfone ketone) as novel stationary phase for stir bar sorptive extraction of organochlorine compounds and organophosphorus pesticides"", 《JOURNAL OF CHROMATOGRAPHY A》, vol. 1177, 1 November 2007 (2007-11-01), XP022392447, DOI: doi:10.1016/j.chroma.2007.10.077 * |
| 朱利平: ""聚醚砜、聚醚砜酮多孔膜的结构可控制备及其表面改性"", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》, no. 2, 15 August 2007 (2007-08-15) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11565193B2 (en) * | 2017-04-11 | 2023-01-31 | Shimadzu Corporation | Component extraction apparatus |
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