CN108159734A - A kind of amino multi-walled carbon nano-tube solid-phase extraction column and preparation method thereof - Google Patents
A kind of amino multi-walled carbon nano-tube solid-phase extraction column and preparation method thereof Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The present invention relates to a kind of amino multi-walled carbon nano-tube solid-phase extraction columns and preparation method thereof.The amino multi-walled carbon nano-tube solid-phase extraction column of the present invention uses packing material of the amino multi-walled carbon nano-tube for solid-phase extraction column, and the amino multi-walled carbon nano-tube is by multi-walled carbon nanotube successively through carboxylated, amination chemistry modification gained.The present invention is mainly suitable for the purification of water fruits and vegetables, tealeaves when edible Residual Pesticides in Farm Produce is measured to sample.Solid-phase extraction column in the present invention has good purification, and the object rate of recovery is high, and cheap, amination modification is simple, the characteristics of being easy to produce in batches.
Description
Technical field
The invention belongs to chemical analysis test technical fields, and in particular to a kind of amino multi-walled carbon nano-tube Solid Phase Extraction
Column and preparation method thereof.
Background technology
Solid phase extraction techniques are in recent years using a kind of relatively broad Sample Pretreatment Technique, which is based on liquid-solid phase
Chromatographic theory, using solid-phase selective absorption and the property selected elution liquid chromatography principle sample is enriched with, detach and
Purification, reaches the separation between sample and matrix interference object.It can be effectively removed in the analysis process by solid phase extraction techniques
The influence of matrix interference object ensures the accuracy and sensitivity of detection.The technology is widely applied to medicine, food and environment inspection
Test detection field.
Multi-walled carbon nanotube is the nanoscale hollow tube that the class graphite plane curling that carbon hexatomic ring is formed forms, and is had good
Chemical stability, thermal stability and high-specific surface area, be a kind of outstanding sorbing material.It is as a kind of new material, closely
Gradually start to be applied in Solid Phase Extraction over year.At present Solid Phase Extraction is being carried out for adsorbent using multi-walled carbon nanotube
It is poor to polar compound adsorption capacity since its structure is single in application process, it is impossible to comprehensive and effective adsorbing base interference
Object limits its clean-up effect.Amino multi-walled carbon nano-tube increases amino on the basis of multi-walled carbon nanotube is original, can be right
Organic acid, polarity pigment and aliphatic acid isopolarity matrix interference object are effectively adsorbed, and can effectively promote the purification to sample
Effect.
Invention content
In view of the problems of the existing technology, it is an object of the invention to design to provide a kind of amino multi-walled carbon nano-tube
The technical solution of solid-phase extraction column and preparation method thereof.
A kind of amino multi-walled carbon nano-tube solid-phase extraction column, it is characterised in that using amination multi-wall carbon nano-tube
The packing material for solid-phase extraction column is managed, the amino multi-walled carbon nano-tube is by multi-walled carbon nanotube successively through carboxylated, amino
Change obtained by chemical modification, chemical modification carries out according to the following steps：
（1）Carboxylated：Multi-walled carbon nanotube is placed in volume ratio as the concentrated sulfuric acid：Concentrated nitric acid=3:In 1 mixed liquor, in 60-70
It flows back 4-6 hours, is cooled to room temperature at DEG C, add in deionized water and wash to neutrality, vacuum is done after crossing 0.45 μm of membrane filtration
It is dry；
（2）Amination：In 110- after multi-walled carbon nanotube, ethylenediamine and dicyclohexylcarbodiimide after carboxylated is mixed
Be heated to reflux at 120 DEG C 24-36 hours, washed after the completion of reaction with absolute ethyl alcohol, cross after 0.45 μm of membrane filtration 60 DEG C it is true
Sky is dry, removes moisture removal completely, obtains amino multi-walled carbon nano-tube.
A kind of amino multi-walled carbon nano-tube solid-phase extraction column, it is characterised in that the amination multi wall carbon is received
The outer diameter of mitron is 8-15 nm, and length is 50 μm；Solid-phase extraction column blank pipe material is high purity polypropylene, and volume is 6 mL；Sieve
Plank matter is high purity polyethylene；Loadings are ± 5 mg of 200 mg, are loaded as 0.7 cm.
The preparation method of the amino multi-walled carbon nano-tube solid-phase extraction column, it is characterised in that include the following steps：
（1）Lower sieve plate is placed in solid-phase extraction column blank pipe bottom；
（2）The amino multi-walled carbon nano-tube filler of 200 mg is put into, solid-phase extraction column side wall is touched, makes filler distribution uniform；
（3）Upper sieve plate is put into solid-phase extraction column, pushes upper sieve plate, filler is compressed, makes filling height in 0.7 cm.
The amino multi-walled carbon nano-tube solid-phase extraction column answering in edible pesticide residue in agricultural products detection
With.
Compared with prior art, the invention has the advantages that：
（1）Amino multi-walled carbon nano-tube solid-phase extraction column provided by the present invention is to sample purification significant effect.It is more traditional solid
Phase extraction column or multi-walled carbon nanotube are the solid-phase extraction column of matrix, the solid-phase extraction column adsorption capacity bigger, can to organic acid,
Polarity pigment and aliphatic acid isopolarity matrix interference object are effectively adsorbed, and effectively promote the clean-up effect to sample；
（2）Amino multi-walled carbon nano-tube solid-phase extraction column preparation method of the present invention is easily operated；
（3）Amino multi-walled carbon nano-tube solid-phase extraction column is at low cost, applied widely, the accuracy and precision of experimental result
Higher level can be reached, be easy to produce in batches and used.
Specific embodiment
It further illustrates the present invention with reference to embodiments.
Embodiment 1：The preparation method of amino multi-walled carbon nano-tube solid-phase extraction column
1）Materials
Take multi-walled carbon nanotube, solid-phase extraction column blank pipe and sieve plate.Wherein the outer diameter of multi-walled carbon nanotube be 8-15 nm, length
It is 50 μm；Solid-phase extraction column blank pipe material is high purity polypropylene, and volume is 6 mL；Sieve plate material is high purity polyethylene.
2）Multi-walled carbon nanotube amination
A carboxylated：Multi-walled carbon nanotube is placed in volume ratio as the concentrated sulfuric acid：Concentrated nitric acid=3:In 1 mixed liquor, at 70 DEG C next time
It flows 4 hours or flows back 6 hours at 60 DEG C, be cooled to room temperature, add in deionized water and wash to neutrality, cross 0.45 μm of filter membrane
It is dried in vacuo after filtering；
B aminations：After multi-walled carbon nanotube, ethylenediamine and dicyclohexylcarbodiimide after carboxylated is mixed at 120 DEG C
It is heated to reflux 24 hours or is heated to reflux at 110 DEG C 36 hours, washed after the completion of reaction with absolute ethyl alcohol, cross 0.45 μm
60 DEG C of vacuum drying, remove moisture removal, obtain amino multi-walled carbon nano-tube completely after membrane filtration.
3）Fill column
Lower sieve plate is placed in solid-phase extraction column blank pipe bottom by a；
B is put into the amino multi-walled carbon nano-tube filler of 200 mg, touches solid-phase extraction column side wall, makes filler distribution uniform；
Upper sieve plate is put into solid-phase extraction column by c, pushes upper sieve plate, is compressed filler, is made filling height in 0.7 cm.
Embodiment 2：Pesticide residue is detected in cucumber
Eight parts of 20g are weighed through the uniform cucumber sample of crushing, stirring in centrifuge tube, wherein six parts add in a concentration of 10 μ g/mL's
50 μ L of α-six six six standard solution, two parts are not added as control, after mixing stands 1 hour, are separately added into 40.0 mL second
Nitrile is homogenized 1 min of extraction in 15000 r/min with homogenizer, 5 g sodium chloride is added in, then be homogenized extraction 1min, by centrifuge tube
Centrifuge is put into, 5min is centrifuged in 3000 r/min, takes 20.0 mL of supernatant, be concentrated into about 2 mL, it is to be clean.
The anhydrous sulphur of about 1cm high is added in amino multi-walled carbon nano-tube solid-phase extraction column made from embodiment 1 respectively
Sour sodium, first with 4 mL acetonitrile-methylbenzene solution before being loaded（3+1, v/v）Prewashing column when liquid level is reached at the top of sodium sulphate, will be treated net
Change sample to be transferred on decontaminating column, then every time with 2 mL acetonitrile-methylbenzene solution（3：1）Sample liquid bottle is washed three times, and by cleaning solution
It is transferred in column.With about 25mL acetonitrile-methylbenzene solution（3：1）Solid-phase extraction column is washed, collects all effluxes in rotary evaporation
In bottle.Spin concentration is done near in 40oC water-baths, is redissolved with n-hexane and is settled to 5.0 mL, is carried out after crossing 0.45 μm of filter membrane
GC-MS is analyzed.
Testing result, which is shown in two parts of control samples, does not detect α-six six six, and α-six six is detected in remaining six parts of mark-on sample
Six recovery of standard addition are between 92.5%-105.1%, relative standard deviation 4.6%.
Embodiment 3：Pesticide residue is detected in tealeaves
Commercially available Longjing tea samples of eight part of 2 g through crushing mixing is weighed in centrifuge tube, wherein six parts add in a concentration of 1 μ g/mL
100 μ L of chlopyrifos standard solution, two parts are not added as control, and mixing stands 1 hour.15 mL acetonitriles are separately added into, are used
Homogenizer is homogenized 1 min of extraction in 15000 r/min, centrifuges 5min in 3000 r/min, takes supernatant in rotary evaporation bottle
In.Sample residue repeats to extract once with 15 mL acetonitriles again respectively, and extracting solution is merged after centrifugation, is concentrated into about 2 mL, treats net
Change.
The anhydrous sulphur of about 1cm high is added in amino multi-walled carbon nano-tube solid-phase extraction column made from embodiment 1 respectively
Sour sodium, first with 4 mL acetonitrile-methylbenzene solution before being loaded（3+1）Prewashing column, when liquid level is reached at the top of sodium sulphate, by sample to be clean
Product are transferred on decontaminating column, then every time with 2 mL acetonitrile-methylbenzene solution（3+1）Sample liquid bottle is washed three times, and cleaning solution is shifted
Enter in column.With about 25mL acetonitrile-methylbenzene solution（3+1）Solid-phase extraction column is washed, collects all effluxes in rotary evaporation bottle.
Spin concentration is done near in 40oC water-baths, is redissolved with n-hexane and is settled to 2.0 mL, and GC-MS is carried out after crossing 0.45 μm of filter membrane
Analysis.
Testing result, which is shown in two parts of control samples, does not detect chlopyrifos, and chlopyrifos is detected in remaining six parts of mark-on sample and is added
The rate of recovery is marked between 90.9%-102.1%, relative standard deviation 5.3%.
Claims (4)
1. a kind of amino multi-walled carbon nano-tube solid-phase extraction column, it is characterised in that use amino multi-walled carbon nano-tube as solid phase
The packing material of extraction column, the amino multi-walled carbon nano-tube are repaiied by multi-walled carbon nanotube through carboxylated, amination chemistry successively
Decorations gained, chemical modification carry out according to the following steps：
（1）Carboxylated：Multi-walled carbon nanotube is placed in volume ratio as the concentrated sulfuric acid：Concentrated nitric acid=3:In 1 mixed liquor, in 60-70
It flows back 4-6 hours, is cooled to room temperature at DEG C, add in deionized water and wash to neutrality, vacuum is done after crossing 0.45 μm of membrane filtration
It is dry；
（2）Amination：In 110- after multi-walled carbon nanotube, ethylenediamine and dicyclohexylcarbodiimide after carboxylated is mixed
Be heated to reflux at 120 DEG C 24-36 hours, washed after the completion of reaction with absolute ethyl alcohol, cross after 0.45 μm of membrane filtration 60 DEG C it is true
Sky is dry, removes moisture removal completely, obtains amino multi-walled carbon nano-tube.
A kind of 2. amino multi-walled carbon nano-tube solid-phase extraction column as described in claim 1, it is characterised in that the amino
The outer diameter of multi-walled carbon nano-tube is 8-15 nm, and length is 50 μm；Solid-phase extraction column blank pipe material is high purity polypropylene, is held
Product is 6 mL；Sieve plate material is high purity polyethylene；Loadings are ± 5 mg of 200 mg, are loaded as 0.7 cm.
3. the preparation method of amino multi-walled carbon nano-tube solid-phase extraction column as claimed in claim 1 or 2, it is characterised in that packet
Include following steps：
（1）Lower sieve plate is placed in solid-phase extraction column blank pipe bottom；
（2）The amino multi-walled carbon nano-tube filler of 200 mg is put into, solid-phase extraction column side wall is touched, makes filler distribution uniform；
（3）Upper sieve plate is put into solid-phase extraction column, pushes upper sieve plate, filler is compressed, makes filling height in 0.7 cm.
4. amino multi-walled carbon nano-tube solid-phase extraction column as claimed in claim 1 or 2 is in edible Residual Pesticides in Farm Produce
Application in amount detection.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745306A (en) * | 2018-06-27 | 2018-11-06 | 东华理工大学 | A kind of preparation method of epoxychloropropane cross-linked chitosan/aminated carbon nano tube composite aerogel |
| CN108889275A (en) * | 2018-08-01 | 2018-11-27 | 东华理工大学 | A kind of preparation method and application at functionalization single angle |
| CN109622011A (en) * | 2018-12-06 | 2019-04-16 | 浙江工业大学 | A kind of amino multi-wall carbon nanotube supported ruthenium catalyst and its preparation and application |
| CN109647001A (en) * | 2018-11-30 | 2019-04-19 | 中国刑事警察学院 | A kind of Furadan carbon nano tube surface molecularly imprinted solid phase extraction column |
| CN110243955A (en) * | 2019-05-20 | 2019-09-17 | 兰韬 | It is exclusively used in the QuEChERS purification pipe and application method of interference component in removal tealeaves and tobacco leaf |
| CN112034079A (en) * | 2020-09-29 | 2020-12-04 | 中国科学院上海营养与健康研究所 | Novel method for detecting aflatoxin content in tea sample |
| CN112229938A (en) * | 2020-11-13 | 2021-01-15 | 上海市农业科学院 | Solid phase extraction column for detecting perfluorinated compounds and manufacturing method and application thereof |
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| CN109647001A (en) * | 2018-11-30 | 2019-04-19 | 中国刑事警察学院 | A kind of Furadan carbon nano tube surface molecularly imprinted solid phase extraction column |
| CN109622011A (en) * | 2018-12-06 | 2019-04-16 | 浙江工业大学 | A kind of amino multi-wall carbon nanotube supported ruthenium catalyst and its preparation and application |
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| CN112034079A (en) * | 2020-09-29 | 2020-12-04 | 中国科学院上海营养与健康研究所 | Novel method for detecting aflatoxin content in tea sample |
| CN112229938A (en) * | 2020-11-13 | 2021-01-15 | 上海市农业科学院 | Solid phase extraction column for detecting perfluorinated compounds and manufacturing method and application thereof |
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Application publication date: 20180615 |