CN104678033A - Filling method of double-layer solid-phase extraction small column and solid-phase extraction small column - Google Patents
Filling method of double-layer solid-phase extraction small column and solid-phase extraction small column Download PDFInfo
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- CN104678033A CN104678033A CN201310618775.0A CN201310618775A CN104678033A CN 104678033 A CN104678033 A CN 104678033A CN 201310618775 A CN201310618775 A CN 201310618775A CN 104678033 A CN104678033 A CN 104678033A
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Abstract
The invention discloses a filling method of a double-layer solid-phase extraction small column and the solid-phase extraction small column. The filling method comprises the steps that firstly, a certain amount of positive-phase adsorption packing or positive-phase bonding packing is weighed, a solid-phase extraction column tube with a screen plate is filled with the certain amount of positive-phase adsorption packing or positive-phase bonding packing, uniform vibration is carried out till a column bed is located at the upper end of the packing in a parallel mode and is fixed through the screen plate, and the column bed serves as a lower layer of the small column; then, a certain amount of water-absorbing packing is weighed, the solid-phase extraction column tube is continuously filled with the water-absorbing packing, uniform vibration is carried out till the column bed is located at the upper end of the water-absorbing material in a parallel mode and is fixed through the screen plate, and the column bed serves as an upper layer of the small column. The double-layer solid-phase extraction small column is filled through a dry method packing mode, and through the method, water impurity in an organic sample can be removed conveniently, and meanwhile, the aim that a sample is separated after passing through the column is achieved; the application range of the solid-phase extraction small column is enlarged, and the number of kinds of adsorption impurities is increased; the method is simple and convenient, filling is easy, and the experiment shows that the double-layer solid-phase extraction small column manufactured through the method is relatively high in extraction efficiency and impurities in filtering products are few.
Description
Technical field
The present invention relates to technical field of analytical chemistry, particularly a kind of packing method of double-deck solid phase extraction column and solid phase extraction column.
Background technology
Solid-Phase Extraction (Solid Phase Extraction is called for short SPE) technology is a kind of sample-pretreating method based on chromatographic resolution.Solid-Phase Extraction comprises solid phase (having the solid adsorbent of certain functional group) and liquid phase (sample and solvent).Fluid sample under the effect of malleation, negative pressure or gravity by being equipped with the solid phase extraction device (solid-phase extraction column, solid-phase extraction membrane, Solid-Phase Extraction suction nozzle, solid-phase extraction chip etc.) of solid adsorbent.Because fixed adsorbent has different functional groups, specific compounds adsorb can be retained on SPE post, thus being separated of realize target thing and magazine.Solid-Phase Extraction can be divided into two kinds of patterns: one is target compound absorption mode Solid-Phase Extraction; Another kind is then impurity absorption pattern Solid-Phase Extraction.
As a Sample Pretreatment Technique, Solid-Phase Extraction is widely used.In some industries, Solid-Phase Extraction replaces traditional liquid-liquid extraction gradually, becomes one of important sample pre-treatments means.Why target compound can be separated by Solid-Phase Extraction from sample substrate, mainly be retained on solid-phase adsorbent by the acting force between the functional group on solid-phase adsorbent and the functional group of target compound by target compound, the sample substrate be not retained then is flowed out by solid phase.This acting force is mainly divided into nonpolar action power, polarity acting force, ionization power, covalent effect power and multi-acting force.
The sample that some matrix are comparatively complicated, after carrying out Solid-Phase Extraction by a kind of filler, still there is the analysis of more impurity jamming target compound, at this moment can consider the method two kinds of extraction stuffings being gathered use, according to the character of impurity and sample, filler can be carried out mixing and load.
Mixing Solid-Phase Extraction mainly by two or more sorptive filler evenly after insert solid-phase extraction column, reach under the prerequisite of not losing target compound, utilize the characteristic of mixing solid-phase extraction column different functional groups, removed the object of sample and heterogeneity chaff interference by the pH value in this adjustment extraction process respectively.
Summary of the invention
The object of the invention is the deficiency for existing method of operating, there is provided a kind of packing method of double-deck solid phase extraction column, the packing method of this double-deck solid phase extraction column not only can ensure the continuity of solid phase extraction sample but also can realize the good production requirement of sample preparation repeatability.
For solving the problems of the technologies described above, the invention provides following technical scheme: a kind of packing method of double-deck solid phase extraction column, first take and just fixing filler and be loaded on and be equipped with in the solid phase extraction tube of sieve plate, fix with sieve plate in upper end after filler vibrations evenly, then water absorptivity filler is taken, filler vibrations are evenly same afterwards to be fixed with sieve plate in upper end, thus forms double-deck solid-phase extraction column.
As a kind of preferred version of the packing method of double-deck solid phase extraction column of the present invention, wherein: its filling step is as follows:
(1) a certain amount of positive sorptive filler or positive bonding filler is taken;
(2) be loaded into and have in the Solid-Phase Extraction column jecket of sieve plate;
(3) vibrations evenly, ensures that post bed is parallel;
(4) mounted sieve is fixed;
(5) a certain amount of water absorptivity filler is taken;
(6) be loaded into and have in the Solid-Phase Extraction column jecket of positive phase filling;
(7) vibrations evenly, ensures that post bed is parallel;
(8) mounted sieve is fixed.
As a kind of preferred version of the packing method of double-deck solid phase extraction column of the present invention, wherein: in described (1), positive phase filling is the one in silica gel, aluminium oxide, zeyssatite, silica gel bonded amino or glycol-based.
As a kind of preferred version of the packing method of double-deck solid phase extraction column of the present invention, wherein: in described (5), water absorptivity filler is the one in calcium oxide, NaOH, anhydrous magnesium sulfate, solid calcium chloride and solid magnesium chloride.
As a kind of preferred version of the packing method of double-deck solid phase extraction column of the present invention, wherein: described positive packing material size is between 60-80 μm.
As a kind of preferred version of the packing method of double-deck solid phase extraction column of the present invention, wherein: described in
Water absorptivity packing material size is between 200-300 order.
Another object of the present invention is to provide a kind of double-deck solid phase extraction column.
A kind of double-deck solid phase extraction column, comprise shell, sieve plate and filler, it is characterized in that: lower floor's filler is positive bonding or adsorption stuffing, upper strata filler is water absorptivity filler.
The invention provides a kind of packing method of double-deck solid phase extraction column, compared with prior art, the present invention adopts dry column-packing to load double-deck solid phase extraction column, and in the convenient organic sample of the method, moisture impurity removal realizes sample simultaneously and crosses post separation; Enriched the range of application of solid phase extraction column, adsorbed impurity species increases; Method is easy, be easy to filling and the double-deck solid phase extraction column utilizing the method to prepare through test prove extraction efficiency higher, in filtration product, impurity is less.
Embodiment
Below in conjunction with specific embodiment, the method for the invention and solid phase extraction column are described in detail.
Be described below in detail embodiments of the invention, the example of described embodiment illustrates, wherein same or similar label represents same or similar composition or has component that is identical or similar functions from start to finish.The following examples are exemplary, only for explaining the present invention, and can not be interpreted as limitation of the present invention.
Embodiment 1
The preparation method of the double-deck solid phase extraction column of glucocorticoid medicine
(1) preparation of the double-deck solid phase extraction column of glucocorticoid medicine:
Take 1 gram of silica filler to be filled in volume and to be 6ml and bottom is equipped with in the polypropylene column jecket of polypropylene sieve plate, vibrations evenly and ensure that post bed is parallel and fix with sieve plate in filler upper end, taking 0.5g anhydrous calcium chloride again fills in column jecket, shakes up to fix with sieve plate equally afterwards.
(2) extract the solid phase extraction column of glucocorticoid, apply and being separated of glucocorticoid medicine, enrichment and purifying:
Take 5g sample pretreating, the sample liquid after transfer processing, to the top of solid-phase extraction column, crosses post with the flow velocity of per second.Merge and collect eluent, filtration treatment analysis, filtrate measures the content of glucocorticoid for liquid chromatography-mass spectrography, and its relative recovery is 84.3%.
Comparative example, only adopts silica gel to be that the individual layer solid-phase extraction column of filler is tested:
Take 5g sample pretreating, the sample liquid after transfer processing, to the top of solid-phase extraction column, crosses post with the flow velocity of per second.Merge and collect eluent, filtration treatment analysis, filtrate measures the content of glucocorticoid for liquid chromatography-mass spectrography, and its relative recovery is 61.8%.
Embodiment 2
The preparation method of the double-deck solid phase extraction column of Gibberella zeae alcohols medicine
(1) preparation of the double-deck solid phase extraction column of Gibberella zeae alcohols medicine:
Take 0.5 gram of bonding alkylamino silica gel filler to be filled in volume and to be 6ml and bottom is equipped with in the polypropylene column jecket of polypropylene sieve plate, vibrations evenly and ensure that post bed is parallel and fix with sieve plate in filler upper end, taking 0.5g anhydrous sodium sulfate again fills in column jecket, shakes up to fix with sieve plate equally afterwards.
(2) being separated of application and Gibberella zeae alcohols medicine of Gibberella zeae alcohols medicine solid phase extraction column, enrichment and purifying: take 5g sample pretreating, the sample liquid after transfer processing, to the top of solid-phase extraction column, crosses post with the flow velocity of per second.Merge and collect eluent, filtration treatment analysis, filtrate measures the content of Gibberella zeae alcohols medicine for liquid chromatography-mass spectrography, and its relative recovery is 86.7%.
Comparative example, only adopts bonding alkylamino silica gel to be that the individual layer solid-phase extraction column of filler is tested:
Take 5g sample pretreating, the sample liquid after transfer processing, to the top of solid-phase extraction column, crosses post with the flow velocity of per second.Merge and collect eluent, filtration treatment analysis, filtrate measures the content of Gibberella zeae alcohols medicine for liquid chromatography-mass spectrography, and its relative recovery is 63.2%.
Embodiment 3
The preparation method of the double-deck solid phase extraction column of carbamate
(1) preparation of the double-deck solid phase extraction column of carbamate:
Take 1 gram of neutral alumina Al filler to be filled in volume and to be 6ml and bottom is equipped with in the polypropylene column jecket of polypropylene sieve plate, vibrations evenly and ensure that post bed is parallel and fix with sieve plate in filler upper end, taking 0.5g lime chloride again fills in column jecket, shakes up to fix with sieve plate equally afterwards.
(2) being separated of application and Gibberella zeae alcohols medicine of carbamate solid phase extraction column, enrichment and purifying: take 5g sample pretreating, the sample liquid after transfer processing, to the top of solid-phase extraction column, crosses post with the flow velocity of per second.Merge and collect eluent, filtration treatment analysis, filtrate sends out mensuration urethane content for chromatography of gases, and its relative recovery is 89.3%.
Comparative example, only adopts neutral alumina to be that the individual layer solid-phase extraction column of filler is tested:
Take 5g sample pretreating, the sample liquid after transfer processing, to the top of solid-phase extraction column, crosses post with the flow velocity of per second.Merge and collect eluent, filtration treatment analysis, filtrate measures the content of carbamate for vapor-phase chromatography method, and its relative recovery is 67.6%.
Claims (6)
1. the packing method of a double-deck solid phase extraction column, concrete grammar is: first take a certain amount of positive sorptive filler or positive bonding filler, be loaded into and have in the Solid-Phase Extraction column jecket of sieve plate, fix with sieve plate in filler upper end after vibrations are evenly parallel to post bed, this is the lower floor of pillar; Then take a certain amount of water absorptivity filler to continue to be loaded in Solid-Phase Extraction column jecket, solid with sieve plate in absorptive substance upper end after vibrations uniform column bed is parallel, this is the upper strata of pillar.
2. the packing method of double-deck solid phase extraction column according to claim 1, is characterized in that:
Its filling step is as follows:
(1) a certain amount of positive sorptive filler or positive bonding filler is taken;
(2) be loaded into and have in the Solid-Phase Extraction column jecket of sieve plate;
(3) vibrations evenly, ensures that post bed is parallel;
(4) mounted sieve is fixed;
(5) a certain amount of water absorptivity filler is taken;
(6) be loaded into and have in the Solid-Phase Extraction column jecket of positive phase filling;
(7) vibrations evenly, ensures that post bed is parallel;
(8) mounted sieve is fixed.
3. the packing method of double-deck solid phase extraction column according to claim 2, is characterized in that, in described step (1), positive phase filling is the one in silica gel, aluminium oxide, zeyssatite, silica gel bonded amino or glycol-based.
4. the packing method of double-deck solid phase extraction column according to claim 2, is characterized in that, in described step (5), water absorptivity filler is the one in calcium oxide, NaOH, anhydrous magnesium sulfate, solid calcium chloride and solid magnesium chloride.
5. the packing method of double-deck solid phase extraction column according to claim 3, is characterized in that: described positive packing material size is between 60-80 μm.
6. the packing method of double-deck solid phase extraction column according to claim 4, is characterized in that: described water absorptivity packing material size is between 200-300 order.
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| CN201310618775.0A CN104678033A (en) | 2013-11-29 | 2013-11-29 | Filling method of double-layer solid-phase extraction small column and solid-phase extraction small column |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106423037A (en) * | 2016-09-13 | 2017-02-22 | 广西大学 | Method for preparing Fe3O4 nanoparticle SPE (Solid Phase Extraction Cartridge) cartridge |
| CN106442080A (en) * | 2016-09-13 | 2017-02-22 | 广西大学 | Method for preparing mixed nano particle SPE column |
| CN109001325A (en) * | 2018-08-08 | 2018-12-14 | 浙江省食品药品检验研究院 | A kind of solid-phase extraction column and its preparation method and application |
| CN110314413A (en) * | 2019-07-30 | 2019-10-11 | 深圳逗点生物技术有限公司 | QuEChERS solid-phase extraction device, preparation method and solid phase extraction method |
| CN111107930A (en) * | 2017-10-18 | 2020-05-05 | 百特基公司 | Sample purification device and method |
-
2013
- 2013-11-29 CN CN201310618775.0A patent/CN104678033A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106423037A (en) * | 2016-09-13 | 2017-02-22 | 广西大学 | Method for preparing Fe3O4 nanoparticle SPE (Solid Phase Extraction Cartridge) cartridge |
| CN106442080A (en) * | 2016-09-13 | 2017-02-22 | 广西大学 | Method for preparing mixed nano particle SPE column |
| CN111107930A (en) * | 2017-10-18 | 2020-05-05 | 百特基公司 | Sample purification device and method |
| CN111107930B (en) * | 2017-10-18 | 2024-03-29 | 百特基公司 | Sample purification apparatus and method |
| CN109001325A (en) * | 2018-08-08 | 2018-12-14 | 浙江省食品药品检验研究院 | A kind of solid-phase extraction column and its preparation method and application |
| CN110314413A (en) * | 2019-07-30 | 2019-10-11 | 深圳逗点生物技术有限公司 | QuEChERS solid-phase extraction device, preparation method and solid phase extraction method |
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Application publication date: 20150603 |