CN107126727A - A kind of nano grain of silver immobilization SPME integral post - Google Patents
A kind of nano grain of silver immobilization SPME integral post Download PDFInfo
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- CN107126727A CN107126727A CN201710558876.1A CN201710558876A CN107126727A CN 107126727 A CN107126727 A CN 107126727A CN 201710558876 A CN201710558876 A CN 201710558876A CN 107126727 A CN107126727 A CN 107126727A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a kind of nano grain of silver immobilization SPME integral post, it is to be used as matrix integral post using mucopolysaccharide functionalization integral post.Nano grain of silver solution is by AgNO3Solution, potassium sodium tartrate solution, sodium citrate solution mix and adjust pH and be made in equal volume, and obtained nano grain of silver is spheric granules of the average grain diameter in 30 nm or so.Nano grain of silver solution is passed through by matrix integral post by Micropump, interacted using sites such as nano grain of silver and matrix integral post surface carboxyl groups, amino, realize the immobilization of nano grain of silver, nano grain of silver immobilization SPME integral post is prepared, and is applied to enrichment and its sequentially eluting of cis-trans-isomer that the unsaturated compound with carbon-carbon double bond is realized in SPME.It is present invention process is simple, easily operated, need not be expensive instrument, easy to spread, and its applicable analysis object range is wide.
Description
Technical field
The invention belongs to integral post preparation field, and in particular to a kind of nano grain of silver immobilization SPME integral post.
Background technology
Integral post is the method by the in-situ polymerization in pipe, a kind of bar-shaped entirety that a step is prepared from, therefore also known as rod
Post.This column type has double-pore structure, and the existing micron order through hole communicated with each other, there is nanoscale again in crosslinking net skeleton
Skeleton hole, causes pillar to hold high-permeability and big specific surface area, efficient, quick, high flux can be reached during as analytical column
With low post pressure.Integral post has the advantages that easily preparation, diversified surface-functionalized, porous and rapid mass transfer due to it,
Lasting concern is attracted in analysis science field.Except traditionally as high performance liquid chromatography (HPLC) and capillary electric chromatogram
(CEC) outside separation stationary phase, integral post is also used for SPE (SPE) or SPME (SPME) before complex sample
Process field shows huge potential.
Nano grain of silver, because it has high conductance, strong bacteriostasis and good photo-catalysis capability etc. outstanding
Performance all receives everybody extensive concern in many fields.The carbon-carbon double bond that nano grain of silver and unsaturated compound are carried it
Between there is special active force, this active force is improved with the increase of double bond quantity, diminished with the growth of carbochain,
The active force of cis unsaturated compound is better than trans unsaturated compound simultaneously.In separation science field, especially integrally
Only have several very few document reports nano grain of silver functionalization integral post answering in chromatographic isolation in post preparation field
With.Zhu et al.（Y. Zhu, et al. J. Sep. Sci., 2015, 38, 2841-2847）Nano grain of silver is derived and arrived
In the macroporous/mesoporous monolithic silica column that aperture structure is optimized, and it is for polycyclic aromatic hydrocarbon and unsaturated with carbon-carbon double bond
The high performance liquid chromatography separation of the cis-trans-isomer of compound.Navarro-Pascual-Ahuir et al.（M. Navarro-
Pascual-Ahuir, et al. Electrophoresis, 2013, 34, 925-934）By ultraviolet light-initiated original position also
Directly the adulterate mode of nano grain of silver solution of former and reaction solution is prepared for the dodecyl methyl propylene of two kinds of doping nano grain of silver
Acid esters integral post, and it is applied to neutral compound（Including the unsaturated compound with carbon-carbon double bond）Capillary electric chromatogram
Separation.However, not yet there is the report that nano grain of silver functionalization integral post is applied in SPME field so far.This hair
It is bright based on the mucopolysaccharide functionalization integral post researched and developed before this seminar, silver is directly realized by by the active function site on its surface
Nanoparticle integral post surface immobilization there is provided a kind of nano grain of silver immobilization SPME integral post new preparation technology,
Promotion and application to nano grain of silver immobilization integral post will bring very big help.
The content of the invention
It is an object of the invention to provide a kind of nano grain of silver immobilization SPME integral post.The present invention is with this problem
The mucopolysaccharide functionalization integral post researched and developed before group is as matrix integral post（Application number：201610816758.1, patent name：
A kind of hydrophilic SPME integral post of mucopolysaccharide functionalization）, and processability is stable, the spherical nano grain of silver of favorable dispersibility
Solution, is aided in down nano grain of silver solution being passed through matrix integral post by Micropump, realizes nano grain of silver immobilization SPME
The preparation of integral post.The active force having benefited between the nano grain of silver of load and the unsaturated compound with carbon-carbon double bond is realized
The enrichment of such compound, and using the difference of such compound cis-trans-isomer force strength, realize that such compound is suitable
The sequentially eluting of trans isomer.
To achieve the above object, the present invention is adopted the following technical scheme that：
First, mucopolysaccharide is uniformly mixed with urea liquid, formalin, catalyst solution, passes through step dehydrating polycondensation in situ
Mucopolysaccharide functionalization integral post is prepared, and as matrix integral post；Average grain diameter is prepared in 30 nm or so, particle size
Distributed area is narrow, performance is stable, favorable dispersibility spherical silver nano-grain；Nano grain of silver solution is passed through base using Micropump
Matter integral post, using the interaction of the carboxyl on matrix integral post surface, amino isoreactivity site and nano grain of silver, realizes that silver is received
The immobilization of the grain of rice；Nano grain of silver immobilization SPME integral post is made.
Wherein, sum is 100% meter by weight percent, and each component accounts for matrix integral post and prepares formula composition gross mass
Percentage is：Mucopolysaccharide 0.1 ~ 1%, urea liquid 38 ~ 52%, formalin 34 ~ 47%, catalyst 7.5 ~ 9.5%.
The mucopolysaccharide is Sodium Hyaluronate or chondroitin sulfate；
The urea liquid, its concentration is 1 g/mL；
The mass concentration of the formalin, wherein formaldehyde is 33% ~ 37%；
The catalyst is hydrochloric acid, and its concentration is 0.20 mol/L；
The nano grain of silver solution, its average grain diameter is in 30 nm or so, and concentration is 1 mmol/L.
The preparation method of described nano grain of silver immobilization SPME integral post, comprises the following steps：
1）The preparation of mucopolysaccharide functionalization integral post：1. Teflon（PTFE）Pipe or polyether-ether-ketone（PEEK）The cleaning of pipe blank pipe：
By PTFE tube（Or PEEK pipes）Liquid phase pump is connected, 10 min, Ran Houtong are rinsed under 0.5 mL/min flow velocitys with Chromatographic Pure Methanol
10 min are dried in nitrogen, the baking oven for being placed in 60 DEG C.2. rapid polycondensation in pipe：Prepared by matrix integral post each in formula
Component is uniformly mixed in appropriate proportion, the quick min of sonic oscillation 1 ~ 2, and then mixture is quickly filled to cleaned drying
PTFE tube（Or PEEK pipes）In, it is closed at both ends and be dipped in the min of heated at constant temperature 10 in 70 DEG C of water-baths；After the completion of question response, with water
For mobile phase, PTFE tube is rinsed on liquid chromatography pump（Or PEEK pipes）The h of solid chromatography column about 1, washes away the molten of the interior residual of bed
Agent and reaction remaining reagent, that is, obtain mucopolysaccharide functionalization integral post（Matrix integral post）.
2）The preparation of nano grain of silver solution：By 1 mmol/L AgNO3Solution, 2.8 mmol/L potassium sodium tartrate solutions, 2
Mmol/L sodium citrate solutions are mixed in equal volume, oscillating ultrasonic, and regulation mixed solution pH value is 10, that is, obtains average grain diameter 30
Nm or so, the nm sections of uv-visible absorption spectroscopy 350 ~ 450 have that obvious absorption peaks, Size Distribution interval are narrow, performance is steady
Fixed, the spherical nano grain of silver solution of 1 mmol/L of favorable dispersibility.
3）The preparation of nano grain of silver immobilization SPME integral post：Before immobilization nano grain of silver, first rinsed with acetonitrile
Matrix integral post, matrix integral post is passed through using Micropump by 1mL nano grain of silver solution, then closed at both ends and be dipped in 70 DEG C of water
The h of heated at constant temperature 2 in bath.After the completion of, using acetonitrile as mobile phase, the h of the integral post about 1 is rinsed on liquid chromatography pump, that is, is obtained
Nano grain of silver immobilization SPME integral post.
The remarkable advantage of the present invention is：
1）The present invention has further played the special performance of mucopolysaccharide functionalization integral post, only need to be simply by nano grain of silver solution
Mucopolysaccharide functionalization integral post is passed through, the active function site on mucopolysaccharide functionalization integral post surface is dexterously make use of, realized
The immobilization of nano grain of silver.Present invention process is simple, easily operated, do not need expensive instrument.
2）Nano grain of silver functionalization prepared by the use local reduction way or direct doping method reported in other work before
In integral post, most nano grain of silver are embedded in integral post matrix, therefore the performance of nano grain of silver can not be obtained
Fully displaying.And the direct immobilization method in surface proposed by the present invention, it can be ensured that the nano grain of silver of immobilization is all in integral post table
Face, is conducive to giving full play to the special performance of nano grain of silver.
3）The present invention prepares matrix integral post and nano grain of silver immobilization substep is carried out, and integral material can be realized respectively
Porosity control and surface chemistry improvement, it is to avoid nano grain of silver solution is to whole in local reduction way or direct doping method
The influence that scapus structure is caused.
4）When the nano grain of silver immobilization SPME integral post that the present invention is provided is applied to SPME, in load sample
During realize the enrichment of unsaturated compound using nano grain of silver and with the special role power between carbon-carbon double bond, and washing
During de-, using the difference of force strength between unsaturated compound cis-trans-isomer and nano grain of silver, realize unsaturated
The sequentially eluting of compound cis-trans-isomer.
Brief description of the drawings
Fig. 1 is the field emission scanning electron microscope figure of nano grain of silver immobilization SPME integral post.
Fig. 2 is mucopolysaccharide functionalization integral material（A）With nano grain of silver immobilization SPME integral material（B）Purple
Outside-visible absorption spectrum figure.
Fig. 3 is, using different integral posts as SPME integral post, to set up In-tube SPME-high performance liquid chromatography
Chromatographic fractionation figure of (In-tube SPME-HPLC) combined system to talan cis-trans-isomer；
A is that, using mucopolysaccharide functionalization integral post as SPME integral post, B is with nano grain of silver immobilization integral post in figure
It is used as SPME integral post.
Fig. 4 is, using different integral posts as SPME integral post, to set up In-tube SPME-HPLC combined systems
To four kinds of cis-trans-isomer mixtures of methyl linoleate（Trans- 9, trans- 12- octadecadienoic acids methyl esters, cis- 9, trans- 12- 18
Carbon dienoic acid methyl ester, trans- 9, cis- 12- octadecadienoic acids methyl esters, cis- 9, cis- 12- octadecadienoic acids methyl esters）Chromatogram point
From figure；
A is that, using mucopolysaccharide functionalization integral post as SPME integral post, B is with nano grain of silver immobilization integral post in figure
It is used as SPME integral post.
Embodiment
In order that content of the present invention easily facilitates understanding, with reference to embodiment to skill of the present invention
Art scheme is described further, but the present invention is not limited only to this.
（1）Mucopolysaccharide functionalization integral post（Matrix integral post）Preparation：1. the cleaning of PTFE tube or PEEK pipe void columns：
It is 750 μm of PTFE tubes by internal diameter（Or PEEK pipes）Liquid phase pump is connected, is rinsed with Chromatographic Pure Methanol under 0.5 mL/min flow velocitys
10 min, remove PTFE tube（Or PEEK pipes）Organic impurities of inwall residual etc., then lead to nitrogen, are placed in 60 DEG C of baking
10 min are dried in case.2. rapid polycondensation in pipe：By 8 mg Sodium Hyaluronates, the g/mL urea liquids of 550 mg 1,450 mg
Formalin, the mol/L hydrochloric acid solutions of 100 mg 0.2 are uniformly mixed, the quick min of sonic oscillation 1 ~ 2, then that mixture is fast
Speed fills the PTFE tube of cleaned drying（Or PEEK pipes）In, it is closed at both ends and be dipped in the min of heated at constant temperature 10 in 70 DEG C of water-baths；
After the completion of question response, using water as mobile phase, PTFE tube is rinsed on liquid chromatography pump（Or PEEK pipes）The h of solid chromatography column about 1,
The solvent of residual and reaction remaining reagent in bed are washed away, that is, obtains mucopolysaccharide functionalization SPME integral post.
（2）The preparation of nano grain of silver solution：By 1 mmol/L AgNO3Solution, 2.8 mmol/L potassium sodium tartrate solutions, 2
Mmol/L sodium citrate solutions are mixed in equal volume, oscillating ultrasonic, and it is 10 to adjust mixed solution pH value with 5 wt% NaOH solutions, i.e.,
Prepare average grain diameter has obvious absorption peaks, chi in 30 nm or so, the nm sections of uv-visible absorption spectroscopy 350 ~ 450
Very little distributed area is narrow, performance stable, the spherical nano grain of silver solution of 1 mmol/L of favorable dispersibility.
（3）The preparation of nano grain of silver immobilization SPME integral post：Before immobilization nano grain of silver, first rinsed with acetonitrile
Matrix integral post, matrix integral post is passed through using Micropump by 1mL nano grain of silver solution, and then integral post is closed at both ends and is dipped in 70
The h of heated at constant temperature 2 in DEG C water-bath.After the completion of, using acetonitrile as mobile phase, the h of the integral post about 1 is rinsed on liquid chromatography pump, i.e.,
Obtain nano grain of silver immobilization SPME integral post.
Application Example 1
Mucopolysaccharide functionalization integral material is prepared as described in above-mentioned embodiment（A）With the micro- extraction of nano grain of silver immobilization solid phase
Take integral material（B）, and uv-visible absorption spectroscopy test is carried out respectively.As shown in Fig. 2 curve A is in ultraviolet-visible light
The nm sections of absorption spectrum 350 ~ 450 do not have absworption peak, and curve B has obvious absorption peaks in 420 nm or so, this absworption peak be by
In the cross-section surface plasma resonance of nano grain of silver, illustrate that nano grain of silver has been immobilized to the overall material of mucopolysaccharide functionalization well
On material.
Application Example 2
Mucopolysaccharide functionalization integral post is prepared as described in above-mentioned embodiment（A）With nano grain of silver immobilization SPME
Integral post（B）, and using both integral posts as SPME integral post, set up In-tube SPME-high-efficient liquid phase color
(In-tube SPME-HPLC) combined system is composed, the SPME behavior of talan cis-trans-isomer is investigated（Fig. 3）.
Specific separation condition：Load sample liquid is constituted：N-hexane/isopropanol=95%/5% (v/v)；Sample solvent：100% just oneself
Alkane；Sample introduction flow velocity：0.1 mL/min；Sampling volume：500 μL；Eluent is constituted：100% n-hexane；Elution flow rate：0.1 mL/
min；Elution volume：150 μL；Separate mobile phase：100% n-hexane；Separate flow velocity：1.0 mL/min；Column oven temperature：30
℃；Detection wavelength：290 nm.In Fig. 3-B, detection peak 1 is cis-stilbene, and detection peak 2 is trans stilbene.
As shown in figure 3, being used as SPME integral post using mucopolysaccharide functionalization integral post（Curve A）When, detect peak
Intensity is relatively low, and talan cis-trans-isomer can not be separated；And nano grain of silver immobilization integral post is used as solid phase
Micro-extraction integral post（Curve B）When, detection peak intensity is strengthened, and talan cis-trans-isomer is separated, and is illustrated
As SPME integral post, nano grain of silver immobilization integral post shows obvious richness to unsaturated compound talan
Collection ability, simultaneously because the active force of trans stilbene and nano grain of silver is better than cis-stilbene, talan cis-trans
Isomers realizes sequentially eluting according to force strength, and is able to efficiently separate analysis, indicates nano grain of silver immobilization solid phase
Micro-extraction integral post has the ability for realizing unsaturated compound cis-trans-isomer sequentially eluting.
Application Example 3
Mucopolysaccharide functionalization integral post is prepared as described in above-mentioned embodiment（A）With nano grain of silver immobilization SPME
Integral post（B）, and using both integral posts as SPME integral post, set up In-tube SPME-high-efficient liquid phase color
(In-tube SPME-HPLC) combined system is composed, four kinds of cis-trans-isomer mixtures of methyl linoleate are investigated（Trans- 9, it is trans-
12- octadecadienoic acids methyl esters, cis- 9, trans- 12- octadecadienoic acids methyl esters, trans- 9, cis- 12- octadecadienoic acids methyl esters,
Cis- 9, cis- 12- octadecadienoic acids methyl esters）SPME behavior（Fig. 4）.
Specific separation condition：Load sample liquid is constituted：N-hexane/isopropanol=95%/5% (v/v)；Sample solvent：100% just oneself
Alkane；Sample introduction flow velocity：0.1 mL/min；Sampling volume：500 μL；Eluent is constituted：100% n-hexane；Elution flow rate：0.1 mL/
min；Elution volume：150 μL；Separate mobile phase：100% n-hexane；Separate flow velocity：1.0 mL/min；Column oven temperature：30
℃；Detection wavelength：203 nm.In Fig. 4-B, detection peak 1 is trans- 9, trans- 12- octadecadienoic acids methyl esters, and detection peak 2,3 is distinguished
It is cis- 9, trans- 12- octadecadienoic acids methyl esters, trans- 9, cis- 12- octadecadienoic acids methyl esters, detection peak 4 is cis- 9, cis-
12- octadecadienoic acid methyl esters.
As shown in figure 4, being used as SPME integral post using mucopolysaccharide functionalization integral post（Curve A）When, detect peak
Intensity is relatively low, and four kinds of cis-trans-isomers of methyl linoleate can not be separated；And use nano grain of silver immobilization integral post to make
For SPME integral post（Curve B）When, detection peak intensity is strengthened, and four kinds of cis-trans-isomers of methyl linoleate are obtained
Separation, illustrates that nano grain of silver immobilization integral post is to unsaturated compound methyl linoleate as SPME integral post
Obvious accumulation ability is shown, simultaneously because four kinds of cis-trans-isomers of methyl linoleate are different from the active force of nano grain of silver,
The cis-structure active force of carbon-carbon double bond is better than transconfiguration, and four kinds of cis-trans-isomers of methyl linoleate are real according to force strength
Existing sequentially eluting, and be able to efficiently separate analysis, indicating nano grain of silver immobilization SPME integral post has realization not
The ability of saturated compounds cis-trans-isomer sequentially eluting.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (7)
1. a kind of nano grain of silver immobilization SPME integral post, it is characterised in that：The integral post is with mucopolysaccharide function
Change integral post as matrix integral post, aid in down nano grain of silver solution being passed through matrix integral post by Micropump, it is whole using matrix
The interaction of the carboxyl on scapus surface, amino avtive spot and nano grain of silver, realizes the immobilization of nano grain of silver, obtained silver is received
Grain of rice immobilization SPME integral post.
2. nano grain of silver immobilization SPME integral post according to claim 1, it is characterised in that：Prepare the entirety
Nano grain of silver used in post exists with granular form, the shape of particle is spherical in shape, average grain diameter is inhaled in 30 nm, ultraviolet-visible light
Receiving the nm sections of spectrum 350 ~ 450 has narrow obvious absorption peaks, Size Distribution interval, performance stabilization, favorable dispersibility.
3. nano grain of silver immobilization SPME integral post according to claim 1 or 2, it is characterised in that：Preparing should
Nano grain of silver solution concentration used in integral post is 1 mmol/L.
4. nano grain of silver immobilization SPME integral post according to claim 1 or 2, it is characterised in that：It is described whole
Scapus is applied to the enrichment that the unsaturated compound with carbon-carbon double bond is realized in SPME.
5. nano grain of silver immobilization SPME integral post according to claim 1 or 2, it is characterised in that：It is described whole
Scapus is applied to the sequentially eluting that the cis-trans-isomer of the unsaturated compound with carbon-carbon double bond is realized in SPME.
6. a kind of method for preparing nano grain of silver immobilization SPME integral post as claimed in claim 1 or 2, its feature
It is：Its preparation process comprises the following steps：
1）The preparation of mucopolysaccharide functionalization SPME integral post：The cleaning, drying of blank pipe is carried out first, then by mucopolysaccharide
Uniformly mix, the quick min of sonic oscillation 1 ~ 2, then mixture quickly filled clean with urea liquid, formalin, catalyst
It is closed at both ends and be dipped in 70 DEG C of water-baths after the completion of the min of heated at constant temperature 10, question response in dry blank pipe, using water as flowing
Phase, integral post is washed off on liquid chromatography pump the solvent of residual in post bed, obtains the mucopolysaccharide functionalization integral post,
It is used as matrix integral post；
2）The preparation of nano grain of silver solution：By 1 mmol/L AgNO3Solution, 2.8 mmol/L potassium sodium tartrate solutions, 2 mmol/
L sodium citrate solutions are mixed in equal volume, and the pH value of regulation mixed solution is 10, that is, obtains nano grain of silver solution；
3）The immobilization of nano grain of silver：Before immobilization nano grain of silver, matrix integral post first is rinsed with acetonitrile, using Micropump by 1mL
Nano grain of silver solution is passed through matrix integral post, then closed at both ends and be dipped in the h of heated at constant temperature 2 in 70 DEG C of water-baths, that is, obtains silver
Nanometer particle fixing SPME integral post.
7. the preparation method of nano grain of silver immobilization SPME integral post according to claim 6, it is characterised in that：
Blank pipe used is teflon pipe or polyether-ether-ketone pipe.
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Cited By (3)
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| CN109030677A (en) * | 2018-07-16 | 2018-12-18 | 福州大学 | A kind of unsaturated compound solid phase micro-extraction method |
| CN110575683A (en) * | 2019-08-29 | 2019-12-17 | 福州佳宸生物科技有限公司 | hydroxyapatite functionalized monolithic column prepared by in-situ mineralization method |
| CN113731379A (en) * | 2021-09-23 | 2021-12-03 | 福州大学 | Silver ion functionalized covalent organic polymer solid-phase extraction column |
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| CN113731379A (en) * | 2021-09-23 | 2021-12-03 | 福州大学 | Silver ion functionalized covalent organic polymer solid-phase extraction column |
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