CN102688749B - Extraction material and preparation method thereof, and device and extraction method used for solid-phase micro-extraction - Google Patents
Extraction material and preparation method thereof, and device and extraction method used for solid-phase micro-extraction Download PDFInfo
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Abstract
The invention provides an extraction material in the following component proportion: that methacrylic acid: ethylene dimethacrylate is 1:1 to 1:8 (in molar ratio); that (methacrylic acid +ethylene dimethacrylate): methanol is 1:5 to 1:40 (in molar ratio); and that the content of azodiisobutyronitrile is 1% to 2% of the total amount of the material (by mass). A preparation method of the extraction material comprises that the above materials are mixed according to the component proportion to form a pre-polymerization solution; that the pre-polymerization solution is processed by ultrasonic and reacts; and that that methanol is introduced into the reacted pre-polymerization solution to remove not reacted reagent. A solid-phase micro-extraction device comprises a draw-off device, an injection device and an extraction tube, wherein two ends of the extraction tube are connected to the draw-off device and the injection device respectively, and the extraction tube is axially equipped with a through hole which is filled with the extraction material. A solid-phase micro-extraction method comprises the steps of preparation, extraction, purification, desorption, and cleaning. According to the invention, the cost is low, and the working efficiency is high.
Description
Technical field
The present invention relates to a kind of fiber material and preparation method, and a kind of device and method for extraction, relate in particular to fiber material and the preparation method in SPME field, and be used for the device and method of SPME.
Background technology
SPME (solid-phase microextraction, SPME) technology is sample pre-treatments and the beneficiation technologies of a novelty of the rise nineties in 20th century, it developed research by the Pawliszyn professor's of Canadian Waterloo university research group in 1989 at first first, belonged to non-solvent selective extraction method.Immerse fiber head in sample solution or head space gas in a period of time, simultaneously agitating solution to accelerate the two alternate speed that reach balance, after ready to balance takes out fiber head and inserts gas-chromatography vaporizer, the material that adsorbs on the thermal desorption coating.Extract imports chromatographic column by mobile phase with it in vaporizer after desorb, the overall process that complete extractions, separation, concentrates.
At present solid-phase micro-extracting device commonly used comprises fiber head or extracting head, handle.Fiber head or extracting head are the vitreous silica fiber heads that the 1cm of an outer casing stainless steel tubule is long, scribble different chromatographic stationary phases or adsorbent, and fiber head is retractable in stainless steel tube, is used for extraction, adsorption sample; Handle is used for installing or the fixed extractor head, can forever use.
But the weak point of existing micro-extraction device is:
(1) the extracting fiber head is subject to operating influence and damages;
(2) the extraction specific area of extracting fiber head is lower;
(3) the import solid-phase micro-extracting device, expensive.
And, use this micro-extraction device, its extracting process also has following deficiency:
(1) extraction yield of infiltration type or head space formula extraction mode is not high;
(2) infiltration type extraction mode, easily the loss fiber head, make fiber head short service life, and production cost is high.
in the SPE field, solid-phase extraction device critical piece commonly used comprises extraction column etc. at present, if directly do SPME with this device, can complete extraction although need not extracting fiber head and high-tension apparatus, but every less important approximately sample solution of hundreds of milliliter that fills in extraction column, during extraction, sample solution is residual many, dead volume is large, desorbed solution concentration is low, simultaneously can't accurate quantification, later stage also need concentrate, the constant volume step just can be completed extraction quantitatively, waste time and energy, troublesome poeration, compare with micro-extraction technique, complex operation is arranged, easily introduce the deficiency of human error.
Summary of the invention
The device and method that main purpose of the present invention is to provide a kind of fiber material and preparation method and is used for SPME solves problems of the prior art and deficiency.
In order to achieve the above object, the invention provides a kind of fiber material, described material is the polymer that obtains by after methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol polymerization reaction take place, and its pre-polymerization fluid component proportioning is as follows: methacrylic acid: GDMA is 1:1～1:8(mol ratio); (methacrylic acid+GDMA): methyl alcohol is 1:5 ~ 1:40(mol ratio); The content of azodiisobutyronitrile is 1%～2%(mass ratio of total amount of material).
The present invention also provides a kind of preparation method of above-mentioned fiber material, and methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol are mixed into pre-polymerization liquid by proportioning; Pre-polymerization liquid is processed through ultrasonic wave and is reacted; Methyl alcohol is passed in reacted pre-polymerization liquid remove unreacted reagent, thereby be extracted material.
With the fiber material that above-mentioned materials and methods is made, porous is better, and permeability is high, specific area is high, adsorption capacity is good.
Further, in the preparation method of described fiber material, ultrasonic power is 40～60W, and the reaction condition of pre-polymerization liquid is to react 1～24 h under 40～80 ℃.
The present invention also provides a kind of solid-phase micro-extracting device, comprises draw-out device, injection device and extracting tube; Described extracting tube one end connects draw-out device, and the other end connects injection device; Described extracting tube axially is provided with a through hole, and is full of above described fiber material in through hole.
Further, described solid-phase micro-extracting device also comprises a sleeve pipe, and described casing pipe sleeve is connected on outside extracting tube.Described sleeve pipe effect is to make extracting tube tightr with being connected of draw-out device, injection device, is difficult for occuring leakage during use.
Further, described solid-phase micro-extracting device, it is characterized in that, described draw-out device comprises injection-tube, piston, piston rod and pushing block, injection-tube axially is provided with a through hole, piston is fixed in piston rod one end, and the piston rod other end is connected with pushing block, piston and injection-tube through-hole wall close contact and can slide in through hole.Its effect is and liquid can be drawn in extracting tube smoothly after injection device coordinates, or discharges from extracting tube.
Further, described solid-phase micro-extracting device is characterized in that, described pushing block is provided with a fixing hole.Its effect is can automatic sampler and whole device is affixed by fixing hole, thereby realizes the extraction process automation.
Further, described solid-phase micro-extracting device is characterized in that, described injection device comprises needle stand and syringe needle, and extracting tube is connected with an end of needle stand, and the needle stand other end and syringe needle are affixed.Its effect is and liquid can be drawn in extracting tube smoothly after draw-out device coordinates, or discharges from extracting tube.
Further, described solid-phase micro-extracting device is characterized in that, described draw-out device and extracting tube junction, described extracting tube and injection device junction are equipped with seal.Its effect is to make the connection between parts tightr, is difficult for occuring leakage during use.
The present invention also provides a kind of solid phase micro-extraction method, adopts above described solid-phase micro-extracting device, and the method comprises the following steps: (1) preparation: extracting tube is filled full with fiber material; (2) extraction: by draw-out device and injection device, sample solution is extracted to extracting tube, and repeatedly aspirate repeatedly; (3) purify: by draw-out device and injection device with air extraction to extracting tube, and suction is repeatedly repeatedly; (4) desorb: by draw-out device and injection device, stripping liquid is extracted to extracting tube, then stripping liquid all is discharged in a container; (5) clean: by draw-out device and injection device, cleaning fluid is extracted to extracting tube, then cleaning fluid is all discharged, and repeatedly aspirate repeatedly; Again by draw-out device and injection device with air extraction to extracting tube, then air is all discharged, and suction is repeatedly repeatedly.
Above described solid-phase micro-extracting device can further include injection-tube, piston, piston rod and pushing block, injection-tube axially is provided with a through hole, piston is fixed in piston rod one end, the piston rod other end is connected with pushing block, piston and injection-tube through-hole wall close contact and can slide in through hole, described pushing block is provided with a fixing hole, and described method is further comprising the steps: the location: by fixing hole, device was fixed on before step (2) is implemented can the automatic sampler of automation mechanized operation on; Off normal: implement install after complete and automatic sampler is separated in step (5).
Further, in described solid phase micro-extraction method step (2), the suction number of times is 20 ~ 40 times, and each draw volume is 200 ~ 400 μ L, and each pumping velocity is 20 ~ 30 μ L/s.
Further, in described solid phase micro-extraction method step (3), the suction number of times is 1 ~ 3 time, and each pumping velocity is 40 ~ 60 μ L/s.
Further, in described solid phase micro-extraction method step (4), suction stripping liquid volume is 100 ~ 300 μ L, and pumping velocity is 20 ~ 30 μ L/s; When discharging stripping liquid, the velocity of discharge is 5 ~ 15 μ L/s.
Further, in described solid phase micro-extraction method step (5), suck purge liquid number of times is 10 ~ 30 times, and each volume is 200 ~ 300 μ L, and pumping velocity is 10 ~ 30 μ L/s; Suction air number of times is 10 ~ 30 times, and pumping velocity is 40 ~ 60 μ L/s.
The invention has the advantages that:
(1) need not to use expensive extracting fiber head, can use under normal pressure, reduce costs, and simple in structure, easy to use;
(2) because fiber material has better porous, permeability is high, specific area is high, and effect of extracting is better;
(3) because apparatus structure is integrated, inner dead volume is little, and desorbed solution is high by the concentration after fiber material, and easily accurate quantitative analysis, need not to pass through concentration step again, reduced extraction step, improved operating efficiency;
(4) can automation mechanized operation, improved operating efficiency.
Description of drawings
Fig. 1 is the structure explosive view of device of the present invention;
Fig. 2 is the generalized section of partial devices of the present invention.
As follows shown in mark in figure: 1, injection-tube; 101, the first through hole; 102, first interface; 2, sleeve pipe; 201, the second through hole; 202, the second interface; 3, extracting tube; 301, third through-hole; 302, the 3rd interface; 4, sealing gasket; 401, fourth hole; 5, needle stand; 501, fifth hole; 6, syringe needle; 7, pushing block; 701, fixing hole; 8, piston rod; 9, piston.
The specific embodiment
This specific embodiment is described further in connection with accompanying drawing.
Embodiment 1:
A kind of fiber material, described material is the polymer that obtains by after methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol polymerization reaction take place, and its pre-polymerization fluid component proportioning is as follows: methacrylic acid: GDMA is the 1:1(mol ratio); (methacrylic acid+GDMA): methyl alcohol is the 1:5(mol ratio); The content of azodiisobutyronitrile is the 1%(mass ratio of total amount of material).
A kind of preparation method of fiber material, methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol are mixed into pre-polymerization liquid by proportioning, pre-polymerization liquid is processed afterreaction through ultrasonic wave, methyl alcohol is passed in reacted pre-polymerization liquid again and remove unreacted reagent, obtain the material for extraction.Wherein ultrasonic power is 40W, and the reaction condition of pre-polymerization liquid is to react 1h under 40 ℃.
As depicted in figs. 1 and 2, a kind of solid-phase micro-extracting device comprises pushing block 7, piston rod 8, piston 9, injection-tube 1, sleeve pipe 2, extracting tube 3, sealing gasket 4, needle stand 5 and syringe needle 6.The affixed piston 9 of piston rod 8 one ends, the affixed pushing block 7 of the other end, pushing block 7 is provided with fixing hole 701; Injection-tube 1, sleeve pipe 2, extracting tube 3, sealing gasket 4 and needle stand 5 longitudinally are respectively equipped with the first through hole 101, the second through hole 201, third through-hole 301, fourth hole 401 and fifth hole 501, and all through holes are communicated with successively; Injection-tube 1 is for being provided with the cylinder of the first through hole 101, and an end is provided with first interface 102, and first interface 102 places are provided with external screw thread; Sleeve pipe 2 is for being provided with the cylinder of the second through hole 201, and an end is provided with the second interface 202, the second interfaces 202 and is provided with internal thread, realizes being spirally connected by first interface 102 and the second interface 202 between injection-tube 1 and sleeve pipe 2; The effect of sleeve pipe 2 is to connect injection-tube 1, and fixed extractor pipe 3, improves the sealing of whole solid-phase micro-extracting device, prevents leakage; Extracting tube 3 is for being provided with the cylinder of third through-hole 301, on extracting tube 3, part is socketed in sleeve pipe 2, and the upper end of extracting tube 3 further is socketed in the first interface 102 of injection-tube 1, and with first interface 102 inwall close contacts, its effect is to prevent that liquid from spilling to the outside internally; The lower end of extracting tube 3 is provided with the 3rd interface 302, the three interfaces 302 and is positioned at outside sleeve pipe 2, and the 3rd interface 302 and sealing gasket 4 close contacts; Sealing gasket 4 is provided with fourth hole 401; Have one to be the fifth hole 501 of inverted "convex" shape in needle stand 5, be divided into large diameter part and little inner-diameter portion whose, sleeve pipe 2 lower ends, extracting tube 3 lower ends and sealing gasket 4 all are socketed in the large diameter part of fifth hole 501, and with fifth hole 501 inwall close contacts; Little inner-diameter portion whose is connected with syringe needle 6.Sleeve pipe 2 lower ends are provided with external screw thread, and the needle stand large diameter partly is provided with internal thread, and sleeve pipe 2 and needle stand 5 are partly realized being spirally connected by sleeve pipe 2 lower ends and needle stand large diameter.
A kind of solid phase micro-extraction method adopts the device for SPME as claimed in claim 1, and the method comprises the following steps:
(1) preparation: extracting tube is filled full with fiber material;
(2) extraction: piston 9 is pushed in injection-tube 1, make between piston 9 and the first through hole 101 inwalls as closely slipping, pushing block 7 is positioned at outside injection-tube 1, can realize pumping liquid; Syringe needle 6 is inserted again and be equipped with in the sample bottle of sample solution, by pull piston 9 in injection-tube 1, make device repeatedly inject suction 20 times, each draw volume is 200 μ L, and pumping velocity is 20 μ L/s;
(3) purify: the syringe needle 6 of described device is moved in the sky sample bottle, and injection suction air is 1 time repeatedly, and pumping velocity is 40 μ L/s;
(4) desorb: the syringe needle 6 of described device is moved in the sample bottle that stripping liquid is housed, aspirate stripping liquid once, draw volume is 100 μ L, and pumping velocity is 20 μ L/s; The syringe needle 6 of described device moves in the liquid phase bottle again, gets stripping liquid, and the speed of getting is 5 μ L/s; Wherein the liquid phase bottle refers to be specifically designed to the sample bottle that chromatography is used, and volume is generally about 2 mL, uses when being used for the chromatographic apparatus sample introduction;
(5) clean: the syringe needle 6 of described device is moved in the sample bottle that cleaning fluid is housed, suction injection 200 μ L totally 10 times repeatedly, and pumping velocity is 10 μ L/s, then the syringe needle 6 of described device is moved in the sky sample bottle, injection suction air is 10 times repeatedly, and pumping velocity is 40 μ L/s.
Embodiment 2:
A kind of fiber material, described material is the polymer that obtains by after methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol polymerization reaction take place, and its pre-polymerization fluid component proportioning is as follows: methacrylic acid: GDMA is the 1:8(mol ratio); (methacrylic acid+GDMA): methyl alcohol is the 1:40(mol ratio); The content of azodiisobutyronitrile is the 2%(mass ratio of total amount of material).
A kind of preparation method of fiber material, methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol are mixed into pre-polymerization liquid by proportioning, pre-polymerization liquid is processed afterreaction through ultrasonic wave, methyl alcohol is passed in reacted pre-polymerization liquid again and remove unreacted reagent, obtain the material for extraction.Wherein ultrasonic power is 60W, and the reaction condition of pre-polymerization liquid is reaction 24 h under 80 ℃.
As depicted in figs. 1 and 2, a kind of device for SPME comprises pushing block 7, piston rod 8, piston 9, injection-tube 1, sleeve pipe 2, extracting tube 3, sealing gasket 4, needle stand 5 and syringe needle 6.The affixed piston 9 of piston rod 8 one ends, the affixed pushing block 7 of the other end, pushing block 7 is provided with fixing hole 701; Injection-tube 1, sleeve pipe 2, extracting tube 3, sealing gasket 4 and needle stand 5 longitudinally are respectively equipped with the first through hole 101, the second through hole 201, third through-hole 301, fourth hole 401 and fifth hole 501, and all through holes are communicated with successively; Injection-tube 1 is for being provided with the cylinder of the first through hole 101, and an end is provided with first interface 102, and first interface 102 places are provided with external screw thread; Sleeve pipe 2 is for being provided with the cylinder of the second through hole 201, and an end is provided with the second interface 202, the second interfaces 202 and is provided with internal thread, realizes being spirally connected by first interface 102 and the second interface 202 between injection-tube 1 and sleeve pipe 2; The effect of sleeve pipe 2 is to connect injection-tube 1, and fixed extractor pipe 3, improves the sealing of whole solid-phase micro-extracting device, prevents leakage; Extracting tube 3 is for being provided with the cylinder of third through-hole 301, on extracting tube 3, part is socketed in sleeve pipe 2, and the upper end of extracting tube 3 further is socketed in the first interface 102 of injection-tube 1, and with first interface 102 inwall close contacts, its effect is to prevent that liquid from spilling to the outside internally; The lower end of extracting tube 3 is provided with the 3rd interface 302, the three interfaces 302 and is positioned at outside sleeve pipe 2, and the 3rd interface 302 and sealing gasket 4 close contacts; Sealing gasket 4 is provided with fourth hole 401; Have one to be the fifth hole 501 of inverted "convex" shape in needle stand 5, be divided into large diameter part and little inner-diameter portion whose, sleeve pipe 2 lower ends, extracting tube 3 lower ends and sealing gasket 4 all are socketed in the large diameter part of fifth hole 501, and with fifth hole 501 inwall close contacts; Little inner-diameter portion whose is connected with syringe needle 6.Sleeve pipe 2 lower ends are provided with external screw thread, and the needle stand large diameter partly is provided with internal thread, and sleeve pipe 2 and needle stand 5 are partly realized being spirally connected by sleeve pipe 2 lower ends and needle stand large diameter.
A kind of solid phase micro-extraction method adopts the device for SPME as claimed in claim 1, and the method comprises the following steps:
(1) preparation: extracting tube is filled full with fiber material;
(2) location: by fixing hole 701 with pushing block 7 be fixed on can the automatic sampler of automation mechanized operation on;
(3) extraction: piston 9 is pushed in injection-tube 1, make between piston 9 and the first through hole 101 inwalls as closely slipping, pushing block 7 is positioned at outside injection-tube 1, can realize pumping liquid; Syringe needle 6 is inserted again and be equipped with in the sample bottle of sample solution, by pull piston 9 in injection-tube 1, make device repeatedly inject suction 40 times, each draw volume is 400 μ L, and pumping velocity is 30 μ L/s;
(4) purify: the syringe needle 6 of described device is moved in the sky sample bottle, and injection suction air is 3 times repeatedly, and pumping velocity is 60 μ L/s;
(5) desorb: the syringe needle 6 of described device is moved in the sample bottle that stripping liquid is housed, aspirate stripping liquid once, draw volume is 300 μ L, and pumping velocity is 30 μ L/s; The syringe needle 6 of described device moves in the liquid phase bottle again, gets stripping liquid, and the speed of getting is 15 μ L/s; Wherein the liquid phase bottle refers to be specifically designed to the sample bottle that chromatography is used, and volume is generally about 2 mL, uses when being used for the chromatographic apparatus sample introduction;
(6) clean: the syringe needle 6 of described device is moved in the sample bottle that cleaning fluid is housed, suction injection 300 μ L totally 30 times repeatedly, and pumping velocity is 30 μ L/s, then the syringe needle 6 of described device is moved in the sky sample bottle, injection suction air is 30 times repeatedly, and pumping velocity is 60 μ L/s.
(7) off normal: pushing block 7 and the automatic sampler of device are separated.
Automatic sampler can be controlled by computer software program, realizes extraction, purification, desorb, the full-automation of cleaning series process.
Embodiment 3:
A kind of fiber material, described material is the polymer that obtains by after methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol polymerization reaction take place, and its pre-polymerization fluid component proportioning is as follows: methacrylic acid: GDMA is the 1:4(mol ratio); (methacrylic acid+GDMA): methyl alcohol is the 1:25(mol ratio); The content of azodiisobutyronitrile is the 1.5%(mass ratio of total amount of material).
A kind of preparation method of fiber material, methacrylic acid, GDMA, azodiisobutyronitrile and methyl alcohol are mixed into pre-polymerization liquid by proportioning, pre-polymerization liquid is processed afterreaction through ultrasonic wave, methyl alcohol is passed in reacted pre-polymerization liquid again and remove unreacted reagent, obtain the material for extraction.Wherein ultrasonic power is 50W, and the reaction condition of pre-polymerization liquid is reaction 14 h under 60 ℃.
The solid-phase micro-extracting device of the present embodiment and method are identical with embodiment 2, and therefore not to repeat here.
The above is only the preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. a solid-phase micro-extracting device, is characterized in that, comprises draw-out device, injection device and extracting tube;
Described extracting tube one end connects draw-out device, and the other end connects injection device;
Described extracting tube axially is provided with a through hole, and is full of fiber material in through hole;
Described draw-out device comprises injection-tube, piston, piston rod and pushing block, and injection-tube axially is provided with a through hole, and piston is fixed in piston rod one end, and the piston rod other end is connected with pushing block, piston and injection-tube through-hole wall close contact and can slide in through hole.
2. solid-phase micro-extracting device according to claim 1, is characterized in that, also comprises a sleeve pipe, and described casing pipe sleeve is connected on outside extracting tube.
3. solid-phase micro-extracting device according to claim 1, is characterized in that, described pushing block is provided with a fixing hole.
4. solid-phase micro-extracting device according to claim 1, is characterized in that, described injection device comprises needle stand and syringe needle, and extracting tube is connected with an end of needle stand, and the needle stand other end and syringe needle are affixed.
5. solid-phase micro-extracting device according to claim 1, is characterized in that, described draw-out device and extracting tube junction, described extracting tube and injection device junction are equipped with seal.
6. a solid phase micro-extraction method, adopt solid-phase micro-extracting device as claimed in claim 3, it is characterized in that,
The method comprises the following steps:
(1) preparation: extracting tube is filled full with fiber material;
(2) extraction: by draw-out device and injection device, sample solution is extracted to extracting tube, and repeatedly aspirate repeatedly;
(3) purify: by draw-out device and injection device with air extraction to extracting tube, and suction is repeatedly repeatedly;
(4) desorb: by draw-out device and injection device, stripping liquid is extracted to extracting tube, then stripping liquid all is discharged in a container;
(5) clean: by draw-out device and injection device, cleaning fluid is extracted to extracting tube, then cleaning fluid is all discharged, and repeatedly aspirate repeatedly; Again by draw-out device and injection device with air extraction to extracting tube, then air is all discharged, and suction is repeatedly repeatedly.
7. solid phase micro-extraction method according to claim 6, it is characterized in that, the solid-phase micro-extracting device that adopts further comprises injection-tube, piston, piston rod and pushing block, injection-tube axially is provided with a through hole, piston is fixed in piston rod one end, and the piston rod other end is connected with pushing block, piston and injection-tube through-hole wall close contact and can slide in through hole, described pushing block is provided with a fixing hole, and described method is further comprising the steps:
The location: by fixing hole, device was fixed on before step (2) is implemented can the automatic sampler of automation mechanized operation on;
Off normal: implement install after complete and automatic sampler is separated in step (5).
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| CN103055540B (en) * | 2012-12-28 | 2015-03-11 | 中国农业大学 | Method for purifying pesticide residues and special purifier thereof |
| CN103316505B (en) * | 2013-07-05 | 2015-04-01 | 上海新拓分析仪器科技有限公司 | Solid-phase micro extraction device and using method of device |
| CN111855257A (en) * | 2020-07-20 | 2020-10-30 | 中山大学 | Solid phase micro-extraction handle suitable for laser fiber |
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| CN2455328Y (en) * | 2000-11-30 | 2001-10-24 | 武汉大学 | Simple solid phase micro-extractor |
| CN2887401Y (en) * | 2005-12-16 | 2007-04-11 | 武汉大学 | Solid phase micro extraction and resolution device |
| CN101148464A (en) * | 2007-11-01 | 2008-03-26 | 上海交通大学 | Method for purifying erythromycin by using molecular engram polymer |
| WO2010087387A1 (en) * | 2009-01-29 | 2010-08-05 | 株式会社日立ハイテクノロジーズ | Device for pretreating sample and mass spectrometer equipped with same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2455328Y (en) * | 2000-11-30 | 2001-10-24 | 武汉大学 | Simple solid phase micro-extractor |
| CN2887401Y (en) * | 2005-12-16 | 2007-04-11 | 武汉大学 | Solid phase micro extraction and resolution device |
| CN101148464A (en) * | 2007-11-01 | 2008-03-26 | 上海交通大学 | Method for purifying erythromycin by using molecular engram polymer |
| WO2010087387A1 (en) * | 2009-01-29 | 2010-08-05 | 株式会社日立ハイテクノロジーズ | Device for pretreating sample and mass spectrometer equipped with same |
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