CN100348289C - Improved solid phase micro extraction method - Google Patents
Improved solid phase micro extraction method Download PDFInfo
- Publication number
- CN100348289C CN100348289C CNB2005100957339A CN200510095733A CN100348289C CN 100348289 C CN100348289 C CN 100348289C CN B2005100957339 A CNB2005100957339 A CN B2005100957339A CN 200510095733 A CN200510095733 A CN 200510095733A CN 100348289 C CN100348289 C CN 100348289C
- Authority
- CN
- China
- Prior art keywords
- solution
- fiber
- phase micro
- solid phase
- extraction method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002470 solid-phase micro-extraction Methods 0.000 title claims description 15
- 239000000835 fiber Substances 0.000 claims abstract description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003993 organochlorine pesticide Substances 0.000 claims abstract description 13
- 239000002798 polar solvent Substances 0.000 claims abstract description 4
- 238000010521 absorption reaction Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N methyl alcohol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- KDCIHNCMPUBDKT-UHFFFAOYSA-N hexane;propan-2-one Chemical compound CC(C)=O.CCCCCC KDCIHNCMPUBDKT-UHFFFAOYSA-N 0.000 claims description 3
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 3
- CMXPERZAMAQXSF-UHFFFAOYSA-M sodium;1,4-bis(2-ethylhexoxy)-1,4-dioxobutane-2-sulfonate;1,8-dihydroxyanthracene-9,10-dione Chemical compound [Na+].O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=CC=C2O.CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC CMXPERZAMAQXSF-UHFFFAOYSA-M 0.000 claims description 3
- 230000007717 exclusion Effects 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 abstract description 20
- 235000013870 dimethyl polysiloxane Nutrition 0.000 abstract description 19
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 abstract description 18
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 abstract description 18
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 238000004458 analytical method Methods 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 239000007790 solid phase Substances 0.000 abstract description 3
- 238000003795 desorption Methods 0.000 abstract 2
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 239000012454 non-polar solvent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- 238000001179 sorption measurement Methods 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 239000011259 mixed solution Substances 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- JLYXXMFPNIAWKQ-GNIYUCBRSA-N gamma-hexachlorocyclohexane Chemical compound Cl[C@H]1[C@H](Cl)[C@@H](Cl)[C@@H](Cl)[C@H](Cl)[C@H]1Cl JLYXXMFPNIAWKQ-GNIYUCBRSA-N 0.000 description 9
- JLYXXMFPNIAWKQ-UHFFFAOYSA-N gamma-hexachlorocyclohexane Natural products ClC1C(Cl)C(Cl)C(Cl)C(Cl)C1Cl JLYXXMFPNIAWKQ-UHFFFAOYSA-N 0.000 description 9
- 229960002809 lindane Drugs 0.000 description 9
- 238000013507 mapping Methods 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- FRCCEHPWNOQAEU-UHFFFAOYSA-N heptachlor Chemical compound ClC1=C(Cl)C2(Cl)C3C=CC(Cl)C3C1(Cl)C2(Cl)Cl FRCCEHPWNOQAEU-UHFFFAOYSA-N 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 238000005192 partition Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 235000020052 applejack Nutrition 0.000 description 2
- FRCCEHPWNOQAEU-LDSHLKOWSA-N cis-heptachlordane Chemical compound ClC1=C(Cl)[C@@]2(Cl)[C@H]3C=C[C@H](Cl)[C@H]3[C@]1(Cl)C2(Cl)Cl FRCCEHPWNOQAEU-LDSHLKOWSA-N 0.000 description 2
- DFBKLUNHFCTMDC-PICURKEMSA-N dieldrin Chemical compound C([C@H]1[C@H]2[C@@]3(Cl)C(Cl)=C([C@]([C@H]22)(Cl)C3(Cl)Cl)Cl)[C@H]2[C@@H]2[C@H]1O2 DFBKLUNHFCTMDC-PICURKEMSA-N 0.000 description 2
- DFBKLUNHFCTMDC-GKRDHZSOSA-N endrin Chemical compound C([C@@H]1[C@H]2[C@@]3(Cl)C(Cl)=C([C@]([C@H]22)(Cl)C3(Cl)Cl)Cl)[C@@H]2[C@H]2[C@@H]1O2 DFBKLUNHFCTMDC-GKRDHZSOSA-N 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- YVGGHNCTFXOJCH-UHFFFAOYSA-N DDT Chemical compound C1=CC(Cl)=CC=C1C(C(Cl)(Cl)Cl)C1=CC=C(Cl)C=C1 YVGGHNCTFXOJCH-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- -1 n-hexane-carrene Chemical compound 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- LCCNCVORNKJIRZ-UHFFFAOYSA-N parathion Chemical compound CCOP(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 LCCNCVORNKJIRZ-UHFFFAOYSA-N 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to an improved solid-phase micro extracting method applied to the analysis of organic substances. The method comprises the following steps: PDMS fiber is immersed in solution A to be tested for more than 2h; solution B which is composed of polar solvent and non-polar solvent is prepared; the PDMS fiber which is absorbed is taken out of the solution A; after the PDMS fiber is dried, the PDMS fiber is immersed in the solution B for more than 1h of desorption; the solution B is blown for constant volume by nitrogen gas, and then, GC-ECD analysis is carried out. The present invention provides an economic, simple and effective solid-phase micro extracting method used for testing organochlorine pesticide in a water body; in a traditional method, the step that fiber is inserted into GC to proceed with thermal desorption is omitted; the method is simple and is easy to be operated; the method is suitable for testing large-scale samples. The traditional method costs 50 dollars, but the method costs less than 10 yuan RMB. The testing limit of the present invention can reach 0.5 ng/L to 45 ng/L, and the recovery rate reaches 80 to 103%; organochlorine pesticide which can be tested has various varieties.
Description
One, technical field
The present invention relates to a kind of improved solid phase micro-extraction method that organic matter is analyzed, a kind of improvement solid phase micro-extraction method that is used to analyze organo-chlorine pesticide of saying so more specifically of being applied to.
Two, background technology
Traditional solid phase micro-extraction method is to measure organic matter with commercial fibre abstraction device, and the SPME of commodity (SPME) equipment very expensive (each extraction is analyzed needs about 50 dollars of costs).The optical fiber that will be used for transfer of data of P.Mayer success is as the fiber of SPME, the general 0.1 dollar of (P.Mayer of each sample of its cost, W.H.J.Vaes, F.Wijnker et al., Sensing dissolved sedimentporewater concentrations of persistent and bioaccumulative pollutants usingdisposable solid-phase microextraction fibers, Environ.Sci.Technol., 34:5177,2000.).Though analysis cost reduces greatly, fiber is inserted the step that pyrolysis is analysed among the GC needs the experimenter that higher operant level is arranged, and wastes time and energy, and is not suitable for large-scale sample determination.
Mentioned in State Intellectual Property Office of the People's Republic of China's invention disclosed patent " analytical method of aroma substance in a kind of applejack " (application number is CN03113273.1) and adopted the higher bipolarity of a kind of sensitivity 75 μ mCarboxen-PDMS extracting head to be used for the detection of applejack aroma substance, when but the PDMS extracting head is used for the first time at 275 ℃ of aging 5h of gas-chromatography injection port, use aging 1h under said temperature for the second time, also need the GC desorb after the extracting head absorption in addition.So not only increase the time of analyzing pre-treatment, also increased disposal cost.
By retrieval find domestic and foreign literature not about this improved solid phase micro-extraction method analyzing organic substance report.
Three, summary of the invention
1. goal of the invention: the purpose of this invention is to provide a kind of little collection method of improved solid phase that can be used for the environment organic pollutant analysis, particularly be applicable to the analysis of organo-chlorine pesticide, can economical, simply, effectively extract the organic matter organo-chlorine pesticide especially in the water body.
2. technical scheme:
Technical scheme of the present invention is:
A kind of improved solid phase micro-extraction method, it may further comprise the steps:
(1) fiber that inner surface is adhered to thick dimethyl silicone polymer (poly-dimethylsiloxane) coating of 15 μ m places more than the solution A 2h to be measured;
(2) prepare the solution B of forming by polar solvent and non-polar solven;
(3) fiber after step (1) absorption is taken out from A solution, dry and be placed in the solution B more than the desorb 1h;
(4) carrying out GC-ECD after with solution B stripping constant volume with nitrogen analyzes.
Inner surface in the step of the present invention (1) adheres to the fiber of thick dimethyl silicone polymer (poly-dimethylsiloxane) coating of 15 μ m, is provided by Fiberguide Industries.It is in order to guarantee the adsorption time of PDMS fiber that the PDMS fiber is placed more than the solution A 2h to be measured, overlong time, and corresponding absorption will reach balance, guarantees that generally adsorption time got final product in 2～3 hours.
Step (2) if in the composition of solution B contain polar solvent and non-polar solven, n-hexane-carrene, n-hexane-acetone, the n-hexane-methyl alcohol of being chosen as commonly used, corresponding volume ratio is 1: 4～4: 1.
Organo-chlorine pesticide in the step (1) comprises lindane, drinox, Niran, DDT, dieldrite, endrin, heptachlor etc., and the minimal detectable concentration of various compositions can reach 0.5～50ng/L, and high concentration can reach hundreds of μ g/L.Be applicable to the mensuration of organo-chlorine pesticide in the true water sample.
Fiber after will adsorbing in the step (3) takes out, and dries to be divided into several segments to the exclusion and to make in its B solution that all is immersed into 0.5～1mL and resolve, and the time is that 1h gets final product.
The length of fiber does not have materially affect for adsorption effect, is chosen as 200mm usually.
3. beneficial effect:
The invention provides a kind of economy of organo-chlorine pesticide in the water body, simple, effective solid phase micro-extraction method measured, save in the conventional method fiber insertion GC is carried out the step that pyrolysis is analysed, method is simple to operation, is adapted to the detection of extensive sample.Traditional method cost needs 50 dollars, and the cost of this method is less than 10 yuans.Detection range of the present invention can reach 0.5-45ng/L, and the rate of recovery reaches 80-103%, and the kind of detectable organo-chlorine pesticide is wide.
Four, the specific embodiment
Below further specify the present invention by example.
Embodiment 1
Accurately prepare the lindane aqueous solution 50mL of 2.5 μ g/L, place the long PDMS fiber of 200mm A solution to adsorb respectively and take out fiber after 30,60,90,120,150,180 minutes, being cut into several sections after drying makes among its n-hexane-carrene that is immersed into 500 μ L (volume ratio is 1: 4) mixed solution B and to resolve 60 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Get its response peak area and adsorption time mapping on chromatogram, lindane reaches partition equilibrium after 120 minutes.
The GC-ECD model is Agilent (Palo Alto, CA, USA) 6890, wherein the detector temperature of gas-chromatography is 280 ℃, chromatographic column is the HP-5 chromatographic column, 30m * 0.32mm * 0.25 μ m, and temperature programming is: 80 ℃-20 ℃/min-220 ℃-30 ℃/min-280 ℃.
Embodiment 2
Accurately prepare the lindane aqueous solution mL of 20 μ g/L, place the long PDMS fiber of 300mm A solution to adsorb respectively and take out fiber after 30,60,90,120,150,180 minutes, being cut into several sections after drying makes among its n-hexane-carrene that is immersed into 500 μ L (volume ratio is 4: 1) mixed solution B and to resolve 60 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Get its response peak area and adsorption time mapping on chromatogram, lindane reaches partition equilibrium after 120 minutes.Chromatographic condition is with embodiment 1.
Embodiment 3
Accurately prepare the heptachlor aqueous solution 50mL of 5 μ g/L, place the long PDMS fiber of 200mm A solution to adsorb respectively and take out fiber after 30,60,90,120,150,180 minutes, being cut into several sections after drying makes among its n-hexane-carrene that is immersed into 500 μ L (volume ratio is 1: 1) mixed solution B and to resolve 60 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Get its response peak area and adsorption time mapping on chromatogram, heptachlor reaches partition equilibrium after 120 minutes.Chromatographic condition is with embodiment 1.
Embodiment 4:
Accurately prepare the lindane water solution A 50mL of 5 μ g/L, place the long PDMS fiber of 200mm the absorption of A solution to take out after 120 minutes, be cut into after drying among several sections mixed solution B that make its n-hexane-carrene that is immersed into 500 μ L (volume ratio is 1: 1) 500 μ L and resolved respectively 15,30,60,90,120 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Get the mapping of its response peak area on chromatogram and adsorption time, resolves that GC-ECD respective peaks area tends towards stability after 60 minutes, so the best parsing time of selection is 60 minutes.Chromatographic condition is with embodiment 1.
Embodiment 5:
Accurately prepare the drinox water solution A 50mL of 30 μ g/L, place the long PDMS fiber of 200mm the absorption of A solution to take out after 120 minutes, being cut into several sections after drying makes among its n-hexane-acetone that is immersed into 1mL (volume ratio is 1: 2) mixed solution B and resolved respectively 15,30,60,90,120 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Get the mapping of its response peak area on chromatogram and adsorption time, resolve that GC-ECD response peak area tends towards stability after 60 minutes.Chromatographic condition is with embodiment 1.
Embodiment 6:
Accurately prepare the lindane water solution A 50mL of 20 μ g/L, place the long PDMS fiber of 200mm the absorption of A solution to take out after 120 minutes, being cut into several sections after drying makes among its n-hexane-methyl alcohol that is immersed into 1mL (volume ratio is 1: 2) mixed solution B and resolved respectively 15,30,60,90,120 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Get the mapping of its response peak area on chromatogram and adsorption time, resolve that GC-ECD respective peaks area tends towards stability after 60 minutes.Chromatographic condition is with embodiment 1.
Embodiment 7:
Accurately the endrin water solution A 50mL of preparation 10 μ g/L places 5,10,15,20,25,30 ℃ of environment to them respectively.Place the long PDMS fiber of 200mm the absorption of A solution to take out after 120 minutes, being cut into several sections after drying makes among its n-hexane-methyl alcohol that is immersed into 1mL (volume ratio is 1: 2) mixed solution B and resolved respectively 60 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Get its response peak area and adsorption time mapping on chromatogram, temperature is not obvious to the peak area response influence.
Embodiment 8:
Really dispose the dieldrite aqueous solution 50mL of five 10 parallel μ g/L with the TAIHU LAKE calibration, place the long PDMS fiber of 200mm the absorption of A solution to take out after 120 minutes, being cut into several sections after drying makes among its n-hexane-carrene that is immersed into 500 μ L (volume ratio is 1: 4) mixed solution B and to resolve 60 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Record detection and be limited to 5ng/L, relative standard deviation is 9.5%, and the rate of recovery is 89%.
Embodiment 9:
Really dispose the lindane aqueous solution 50mL of five 20 parallel μ g/L with the TAIHU LAKE calibration, place the long PDMS fiber of 200mm the absorption of A solution to take out after 120 minutes, being cut into several sections after drying makes among its n-hexane-carrene that is immersed into 600 μ L (volume ratio is 4: 1) mixed solution B and to resolve 60 minutes, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Record detection and be limited to 21ng/L, relative standard deviation is 0.87%, and the rate of recovery is 82%.
Embodiment 10:
Be respectively the lindane aqueous solution 50mL of 2.5,5,10,20,40 μ g/L with Taihu Lake water sample preparation qualifying concentration, respectively wherein with the submergence of 200mm fiber, after the absorption of 120 clocks, take out, resolved 60 minutes in n-hexane-carrene (volume ratio is 1: 1) mixed solution of adding 500 μ L after drying, slowly blow away solvent with pure nitrogen, constant volume enters GC-ECD and analyzes to 200 μ L.Its concentration and peak area response present good linear relationship R=0.993.
The optimal parameter of determining this method from embodiment is: adsorption time 120min, resolve time 60min.For simplicity, choose room temperature and be test temperature for 25 ℃.This method can reach 0.5-45ng/L to the LDL of organo-chlorine pesticide, and the rate of recovery reaches 80-103%.
With improved solid phase micro-extraction method the organo-chlorine pesticide in the water sample of Taihu Lake is detected.Result and other laboratories that this method is measured compare with the measured data of traditional SPE (SPE) method, find that the result is very identical.This illustrates that improved solid phase micro-extraction method is simple, economical, effective, can be used for large-scale Analysis of environmental samples.The present invention also can be used for other relevant organic analyses, is not limited to the analysis of organo-chlorine pesticide, as long as character is fit to the absorption of PDMS fiber, can select other method for chromatographic determination.
Claims (4)
1, a kind of improved solid phase micro-extraction method is characterized in that may further comprise the steps:
(1) fiber that inner surface is adhered to the thick dimethyl silicone polymer coating of 15 μ m places more than the solution A 2h to be measured;
(2) prepare the solution B of forming by polar solvent and non-polar solven;
(3) fiber after step (1) absorption is taken out from A solution, dry to be placed on and resolve more than the 1h in the solution B;
(4) carrying out GC-ECD after with solution B stripping constant volume with nitrogen analyzes.
2, a kind of improved solid phase micro-extraction method according to claim 1 is characterized in that the least concentration of the various compositions of the organo-chlorine pesticide that contains in the solution to be measured in the step (1) can be 5-45ng/L.
3, a kind of improved solid phase micro-extraction method according to claim 2 is characterized in that the composition of the solution B in the step (2) can be n-hexane-carrene, n-hexane-acetone, n-hexane-methyl alcohol, and corresponding volume ratio is 1: 4～4: 1.
4, a kind of improved solid phase micro-extraction method according to claim 3, fiber after it is characterized in that will adsorbing in the step (3) takes out, dry and be divided into several segments to the exclusion and make in its B solution that all is immersed into 0.5～1m L and resolve, the time is 1h～2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100957339A CN100348289C (en) | 2005-11-18 | 2005-11-18 | Improved solid phase micro extraction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100957339A CN100348289C (en) | 2005-11-18 | 2005-11-18 | Improved solid phase micro extraction method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1785475A CN1785475A (en) | 2006-06-14 |
| CN100348289C true CN100348289C (en) | 2007-11-14 |
Family
ID=36783139
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100957339A Expired - Fee Related CN100348289C (en) | 2005-11-18 | 2005-11-18 | Improved solid phase micro extraction method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100348289C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109001351A (en) * | 2017-12-12 | 2018-12-14 | 东莞理工学院 | A kind of method that magnetic Nano graphene analyzes pre-treatment for polycyclic aromatic hydrocarbon in water body and organo-chlorine pesticide |
| CN114504842B (en) * | 2022-03-02 | 2023-05-26 | 郑州大学第一附属医院 | Cotton fiber support liquid phase extraction device and application thereof in drug concentration detection |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0794822A1 (en) * | 1995-09-28 | 1997-09-17 | Varian Associates, Inc. | Solid phase microextraction with vibration |
| CN1444041A (en) * | 2003-04-22 | 2003-09-24 | 江南大学 | Method for analyzing fragrancer matter in apple wine |
-
2005
- 2005-11-18 CN CNB2005100957339A patent/CN100348289C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0794822A1 (en) * | 1995-09-28 | 1997-09-17 | Varian Associates, Inc. | Solid phase microextraction with vibration |
| CN1444041A (en) * | 2003-04-22 | 2003-09-24 | 江南大学 | Method for analyzing fragrancer matter in apple wine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1785475A (en) | 2006-06-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Majchrzak et al. | PTR-MS and GC-MS as complementary techniques for analysis of volatiles: A tutorial review | |
| Li et al. | Molecularly imprinted calixarene fiber for solid-phase microextraction of four organophosphorous pesticides in fruits | |
| Pawliszyn | New directions in sample preparation for analysis of organic compounds | |
| Wu et al. | Determination of stimulants in human urine and hair samples by polypyrrole coated capillary in-tube solid phase microextraction coupled with liquid chromatography-electrospray mass spectrometry | |
| Santos et al. | Application of solid-phase microextraction to the analysis of volatile organic compounds in water | |
| Regert et al. | Molecular characterisation of birch bark tar by headspace solid-phase microextraction gas chromatography–mass spectrometry: A new way for identifying archaeological glues | |
| Yassaa et al. | Enantiomeric monoterpene emissions from natural and damaged Scots pine in a boreal coniferous forest measured using solid-phase microextraction and gas chromatography/mass spectrometry | |
| Liu et al. | Determination of carbamate and organophosphorus pesticides in fruits and vegetables using liquid chromatography-mass spectrometry with dispersive solid phase extraction | |
| Watson et al. | Air monitoring: New advances in sampling and detection | |
| Vaz | Screening direct analysis of PAHS in atmospheric particulate matter with SPME | |
| Turner et al. | Gas Chromatography–Mass Spectrometry: How Do I Get the Best Results? | |
| CN100348289C (en) | Improved solid phase micro extraction method | |
| Oh et al. | Rapid determination of floral aroma compounds of lilac blossom by fast gas chromatography combined with surface acoustic wave sensor | |
| Ketola et al. | Detection of volatile organic compounds by temperature-programmed desorption combined with mass spectrometry and Fourier transform infrared spectroscopy | |
| Matisová et al. | Solid‐phase microextraction of volatile polar compounds in water | |
| CN102095809A (en) | Analysis method for detecting pyrazine compounds in beer | |
| Aguilar et al. | On-line coupling of equilibrium-sorptive enrichment to gas chromatography to determine low-molecular-mass pollutants in environmental water samples | |
| Saba et al. | A simple method for the extraction of volatile organic compounds contained in air samples from adsorbent materials by solid phase microextraction and their analysis by gas chromatography/mass spectrometry | |
| Cappiello et al. | Application of nano-FIA-Direct-EI-MS to determine diethylene glycol in produced formation water discharges and seawater samples | |
| Kraleva et al. | Determination of PAH in the black sea water by GC/MS following preconcentration with solid-phase extraction | |
| Nakashima et al. | Volatile organic compound (VOC) analysis and anti-VOC measures in water-based paints | |
| CN110579557B (en) | HPLC analysis detection method for simultaneously detecting 12 monocyclic aromatic hydrocarbons in water | |
| Bauer et al. | Acrolein dimer as a marker for direct detection of acrolein in wine | |
| Zabiegała et al. | Application of the chromatographic retention index system for the estimation of the calibration constants of permeation passive samplers with polydimethylsiloxane membranes | |
| Thomas et al. | The applicability of field-portable GC–MS for the rapid sampling and measurement of high-boiling-point semivolatile organic compounds in environmental samples |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20071114 Termination date: 20111118 |