CN103239889A - Filling method of small solid-phase extraction column with mixed packing, and small solid-phase extraction column - Google Patents
Filling method of small solid-phase extraction column with mixed packing, and small solid-phase extraction column Download PDFInfo
- Publication number
- CN103239889A CN103239889A CN2013101536581A CN201310153658A CN103239889A CN 103239889 A CN103239889 A CN 103239889A CN 2013101536581 A CN2013101536581 A CN 2013101536581A CN 201310153658 A CN201310153658 A CN 201310153658A CN 103239889 A CN103239889 A CN 103239889A
- Authority
- CN
- China
- Prior art keywords
- phase extraction
- extraction column
- filler
- solid phase
- packing
- 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.)
- Granted
Links
Abstract
The invention discloses a filling method of a small solid-phase extraction column with mixed packing, and the small solid-phase extraction column. The filling method comprises the following steps: respectively weighing reverse-phase bonded silica gel adsorbent packing and/or inorganic substrate packing; evenly mixing in a rotary self-mixing mode and filling into the small column with a sieve plate; and fixing the sieve plate on the upper end of the packing. According to the method, the small solid-phase extraction column with the mixed packing is filled by using the dry method; and the multiple kinds of packing are evenly mixed in the rotary self-mixing mode before the column is filled, so that the packing can be evenly distributed in the small solid-phase extraction column; and the repeatability of the treated product is good. Therefore, the application range of the small solid-phase extraction column is enlarged, i.e., the small solid-phase extraction column can be used for adsorbing more kinds of impurities. The method is simple and convenient and easy in filling operation. The experiment shows that the small solid-phase extraction column prepared by using the method is higher in efficiency and resulted in fewer impurities in a filtering product.
Description
Technical field
The present invention relates to technical field of analytical chemistry, particularly a kind of solid phase extraction column preparation method of mixed fillers and the solid phase extraction column that utilizes this loading method to load.
Background technology
SPE (solid phase extraction is called for short SPE) is a kind of sample-pretreating method based on chromatographic isolation.SPE comprises solid phase (solid absorbent with certain functional group) and liquid phase (sample and solvent).Fluid sample is the solid phase extraction device (solid-phase extraction column, solid-phase extraction membrane, SPE suction nozzle, solid-phase extraction chip etc.) by solid absorbent is housed under the effect of malleation, negative pressure or gravity.Because solid absorbent has different functional groups, can and be retained on the SPE post specific compound absorption, thereby realize object and separate impurities.SPE can be divided into two kinds of patterns: a kind of is the SPE of target compound absorption mode; Another kind then is the SPE of impurity absorption pattern.
As a sample pre-treatments technology, SPE is widely used.In some industries, SPE replaces traditional liquid-liquid extraction gradually, becomes one of important sample pre-treatments means.Why solid-phase extraction device can be separated target compound from sample substrate, mainly be by the active force between the functional group of the functional group on the solid-phase adsorbent and target compound target compound to be retained on the solid-phase adsorbent, the sample substrate that is not retained then passes through solid-phase extraction device.This active force mainly is divided into nonpolar action power, polarity active force, ionization power, covalent effect power and multiple active force.
Some matrix are complicated sample comparatively, after carrying out SPE by a kind of filler, more impurity interference is still arranged to the analysis of target compound, at this moment, can consider two kinds of extraction stuffings are combined use and the method for combination, according to the character of impurity and sample, filler can be carried out layering and load (multidimensional extraction) or mix filling.
Mix the SPE material and mainly be and insert solid-phase extraction column after two kinds or two or more sorbing material mixed, reach under the prerequisite of not losing target compound, the characteristic of utilize mixing the solid-phase extraction column different functional groups, by regulate pH value in the extraction process remove respectively sample and among the purpose of heterogeneity chaff interference.Accordingly, solid phase extraction column is the prevailing solid-phase extraction device that can buy in each big instrument company at present.The SPE pillar is made up of three parts: filler, porous polypropylene sieve plate and polypropylene for medical article column jecket.
Mostly by abroad being grasped, research mixes the loading method of solid phase extraction column and utilizes the solid phase extraction column of this loading method preparation just to become problem demanding prompt solution for domestic used solid phase extraction column and correlation technique at present.
Summary of the invention
The purpose of this part is to summarize some aspects of embodiments of the invention and briefly introduces some preferred embodiments.In this part and the application's specification digest and denomination of invention, may do a little simplification or omit to avoid making the purpose of this part, specification digest and denomination of invention fuzzy, and this simplification or omit and can not be used for limiting the scope of the invention.
Problem in view of existing in the packing method of above-mentioned and/or existing mixed fillers solid phase extraction column and the preparation solid phase extraction column has proposed the present invention.
Therefore, one of them purpose of the present invention is the deficiency at existing method of operating, a kind of packing method of mixed fillers solid phase extraction column is provided, the packing method of this mixed fillers solid phase extraction column both can guarantee uniform filling in the solid phase extraction column, can realize handling the production requirement of sample good reproducibility again.
For solving the problems of the technologies described above, the invention provides following technical scheme: a kind of packing method of mixed fillers solid phase extraction column, take by weighing reversed-phase bonded silica adsorbent filler and/or inorganic matrix filler respectively, use rotation to mix from the mode of mixing and be loaded in the pillar with sieve plate, the filler upper end is fixed with sieve plate again.
As a kind of preferred version of the packing method of mixed fillers solid phase extraction column of the present invention, wherein: its filling step is as follows: a) take by weighing reversed-phase bonded silica adsorbent filler and inorganic matrix filler respectively; B) adopt rotation from the mode of mixing above-mentioned two kinds of fillers to be mixed; The filler that c) will mix adopts dry column-packing to be loaded in the solid phase extraction column closely; B) mounted sieve is fixed.
As a kind of preferred version of the packing method of mixed fillers solid phase extraction column of the present invention, wherein: reversed-phase bonded silica adsorbent filler is to be selected from least a in carbon 18, carbon eight, carbon four, the carbon two in the described step a).
As a kind of preferred version of the packing method of mixed fillers solid phase extraction column of the present invention, wherein: described its particle diameter of reversed-phase bonded silica adsorbent filler is between 55 μ m～70 μ m.
As a kind of preferred version of the packing method of mixed fillers solid phase extraction column of the present invention, wherein: the inorganic matrix filler is to be selected from least a in silica gel, aluminium oxide, zirconia, the titanium oxide in the described step a).
As a kind of preferred version of the packing method of mixed fillers solid phase extraction column of the present invention, wherein: described its particle diameter of inorganic matrix filler is between 100～200 orders.
As a kind of preferred version of the packing method of mixed fillers solid phase extraction column of the present invention, wherein: rotation is to mix 20 minutes under the rotating speed of 2-3rpm from the mode of mixing in the described step b).
As a kind of preferred version of the packing method of mixed fillers solid phase extraction column of the present invention, wherein: the weight ratio of described reversed-phase bonded silica adsorbent filler and inorganic matrix filler is 1:0.5～1:1.5.
Another object of the present invention provides a kind of mixed fillers solid phase extraction column.
A kind of mixed fillers solid phase extraction column comprises shell, sieve plate and filler, it is characterized in that: described filler is reversed-phase bonded silica adsorbent filler and inorganic matrix filler.
As a kind of preferred version of mixed fillers solid phase extraction column of the present invention, wherein: described reversed-phase bonded silica adsorbent filler is carbon 18, and described inorganic matrix filler is aluminium oxide.
The invention provides a kind of packing method of mixed fillers solid phase extraction column, compared with prior art, the present invention adopts dry column-packing to load mixed fillers solid phase extraction pillar, and uses before loading and rotate from the mode of mixing multiple filler mixing mixing.This process can guarantee uniform filling in the solid phase extraction column, handles the sample good reproducibility; Enriched the range of application of solid phase extraction column, the absorption dopant species increases; Method is easy, is easy to load and utilizes the solid phase extraction column of the method preparation higher through the evidence extraction efficiency, and impurity still less in the filtration product.
The specific embodiment
Below in conjunction with specific embodiment the method for the invention and device are elaborated.
Describe embodiments of the invention below in detail, the example of described embodiment illustrates, and wherein identical or similar label is represented identical or similar composition or had the component of identical or similar functions from start to finish.The following examples are exemplary, only are used for explaining the present invention, and can not be interpreted as limitation of the present invention.
Embodiment 1
One, the preparation method of the solid phase extraction column of pterostilbene:
(1) preparation of the filler of extraction pterostilbene:
Take by weighing 1g55 micron C respectively
18With 0.5g100 order Al
2O
3, fully mix Uniform.Two kinds of fillers that take by weighing are poured in the round-bottomed flask, used Rotary Evaporators under the rotating speed of 2rpm, to mix 20 minutes.
(2) preparation of the solid phase extraction column of extraction pterostilbene:
Take by weighing the above-mentioned filler of 1.5g, being filled in the bottom is in the polypropylene pillar of polyethylene sieve plate, and the filler upper end is fixed with the polyethylene sieve plate again.
Two, extract the solid phase extraction column of pterostilbene, be applied to separation, enrichment and the purifying of pterostilbene:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of pterostilbene, and the relative recovery of pterostilbene is 89.3%.
Comparative Examples only adopts C
18Load for filler and without loading method of the present invention:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of pterostilbene, and the relative recovery of pterostilbene is 62.5%.
Embodiment 2
One, the preparation method of the solid phase extraction column of white skin China fir alcohol:
(1) preparation of the filler of the white skin China fir alcohol of extraction:
Take by weighing 1g60 micron C respectively
18With 1g150 order Al
2O
3, fully mix Uniform.Two kinds of fillers that take by weighing are poured in the round-bottomed flask, used Rotary Evaporators under the rotating speed of 3rpm, to mix 20 minutes.
(2) preparation of the solid phase extraction column of the white skin China fir alcohol of extraction:
Take by weighing the above-mentioned filler of 1g, being filled in the bottom is in the polypropylene pillar of polyethylene sieve plate, and the filler upper end is fixed with the polyethylene sieve plate again.
Two, extract the solid phase extraction column of white skin China fir alcohol, be applied to separation, enrichment and the purifying of white skin China fir alcohol:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of white skin China fir alcohol, and the relative recovery of white skin China fir alcohol is 82.7%.
Comparative Examples only adopts Al
2O
3Load for filler and without loading method of the present invention:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of white skin China fir alcohol, and the relative recovery of white skin China fir alcohol is 67.3%.
Embodiment 3
One, the preparation method of the solid phase extraction column of resveratrol:
(1) preparation of the filler of extraction resveratrol:
Take by weighing 1g70 micron C respectively
18With 1.5g200 order Al
2O
3, fully mix Uniform.Two kinds of fillers that take by weighing are poured in the round-bottomed flask, used Rotary Evaporators under the rotating speed of 3rpm, to mix 20 minutes.
(2) preparation of the solid phase extraction column of extraction resveratrol:
Take by weighing the above-mentioned filler of 1g, being filled in the bottom is in the polypropylene pillar of polyethylene sieve plate, and the filler upper end is fixed with the polyethylene sieve plate again.
Two, extract the solid phase extraction column of resveratrol, be applied to separation, enrichment and the purifying of resveratrol:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of resveratrol, and the relative recovery of resveratrol is 78.5%.
Comparative Examples only adopts Al
2O
3Load for filler and without loading method of the present invention:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of resveratrol, and the relative recovery of resveratrol is 61.2%.
Embodiment 4
One, the preparation method of the solid phase extraction column of pterostilbene:
(1) preparation of the filler of extraction pterostilbene:
Take by weighing 1g55 micron C respectively
18With 1g150 order Al
2O
3, fully mix Uniform.Two kinds of fillers that take by weighing are poured in the round-bottomed flask, used Rotary Evaporators under the rotating speed of 2rpm, to mix 20 minutes.
(2) preparation of the solid phase extraction column of extraction pterostilbene:
Take by weighing the above-mentioned filler of 1g, being filled in the bottom is in the polypropylene pillar of polyethylene sieve plate, and the filler upper end is fixed with the polyethylene sieve plate again.
Two, extract the solid phase extraction column of pterostilbene, be applied to separation, enrichment and the purifying of pterostilbene:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of pterostilbene, and the relative recovery of pterostilbene is 90.6%.
Comparative Examples adopts C
18And Al
2O
3Load for filler and without loading method of the present invention:
Take by weighing the 2g sample and handle, the sample liquid after the transfer processing is crossed post to the top of solid-phase extraction column with the flow velocity of one of per second.Merge and collect eluent, the filtration treatment analysis, filtrate feed flow phase chromatography-mass spectroscopy is measured the content of pterostilbene, and the relative recovery of pterostilbene is 68.3%.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
1. the packing method of a mixed fillers solid phase extraction column, it is characterized in that: take by weighing reversed-phase bonded silica adsorbent filler and/or inorganic matrix filler respectively, use rotation to mix from the mode of mixing and be loaded in the pillar with sieve plate, the filler upper end is fixed with sieve plate again.
2. the packing method of mixed fillers solid phase extraction column according to claim 1 is characterized in that:
Its filling step is as follows:
A) take by weighing reversed-phase bonded silica adsorbent filler and inorganic matrix filler respectively;
B) adopt rotation from the mode of mixing above-mentioned two kinds of fillers to be mixed;
The filler that c) will mix adopts dry column-packing to be loaded in the solid phase extraction column closely;
B) mounted sieve is fixed.
3. the packing method of mixed fillers solid phase extraction column according to claim 2 is characterized in that: reversed-phase bonded silica adsorbent filler is to be selected from least a in carbon 18, carbon eight, carbon four, the carbon two in the described step a).
4. the packing method of mixed fillers solid phase extraction column according to claim 3, it is characterized in that: described its particle diameter of reversed-phase bonded silica adsorbent filler is between 55 μ m～70 μ m.
5. the packing method of mixed fillers solid phase extraction column according to claim 2 is characterized in that: the inorganic matrix filler is to be selected from least a in silica gel, aluminium oxide, zirconia, the titanium oxide in the described step a).
6. the packing method of mixed fillers solid phase extraction column according to claim 5, it is characterized in that: described its particle diameter of inorganic matrix filler is between 100～200 orders.
7. the packing method of mixed fillers solid phase extraction column according to claim 2 is characterized in that: rotation is to mix 20 minutes under the rotating speed of 2-3rpm from the mode of mixing in the described step b).
8. according to the packing method of the arbitrary described mixed fillers solid phase extraction column of claim 2-6, it is characterized in that: the weight ratio of described reversed-phase bonded silica adsorbent filler and inorganic matrix filler is 1:0.5～1:1.5.
9. the solid phase extraction column loaded of packing method according to claim 1 comprises shell, sieve plate and filler, and it is characterized in that: described filler is reversed-phase bonded silica adsorbent filler and inorganic matrix filler.
10. solid phase extraction column according to claim 9, it is characterized in that: described reversed-phase bonded silica adsorbent filler is carbon 18, and described inorganic matrix filler is aluminium oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310153658.1A CN103239889B (en) | 2013-04-27 | 2013-04-27 | Filling method of small solid-phase extraction column with mixed packing, and small solid-phase extraction column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310153658.1A CN103239889B (en) | 2013-04-27 | 2013-04-27 | Filling method of small solid-phase extraction column with mixed packing, and small solid-phase extraction column |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103239889A true CN103239889A (en) | 2013-08-14 |
| CN103239889B CN103239889B (en) | 2015-04-15 |
Family
ID=48919982
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310153658.1A Active CN103239889B (en) | 2013-04-27 | 2013-04-27 | Filling method of small solid-phase extraction column with mixed packing, and small solid-phase extraction column |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103239889B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110455943A (en) * | 2019-07-25 | 2019-11-15 | 苏州艾迪迈医疗科技有限公司 | A kind of on-line mixing filler solid-phase extraction column and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10300739A (en) * | 1997-05-01 | 1998-11-13 | Fuji Spinning Co Ltd | Manufacture of cartridge filling column for solid-phase extraction |
| CN1803242A (en) * | 2005-11-29 | 2006-07-19 | 林黎明 | Solid phase dispersion microwave extraction method of sample residues matrix and extraction stuffing and solvent |
| CN102049151A (en) * | 2009-10-28 | 2011-05-11 | 中国医学科学院药用植物研究所 | Solid phase extraction column for patulin |
| CN102507805A (en) * | 2011-10-27 | 2012-06-20 | 湖南省产商品质量监督检验院 | Method for detecting trichothecene compound in grain and solid phase extraction column for detection |
-
2013
- 2013-04-27 CN CN201310153658.1A patent/CN103239889B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10300739A (en) * | 1997-05-01 | 1998-11-13 | Fuji Spinning Co Ltd | Manufacture of cartridge filling column for solid-phase extraction |
| CN1803242A (en) * | 2005-11-29 | 2006-07-19 | 林黎明 | Solid phase dispersion microwave extraction method of sample residues matrix and extraction stuffing and solvent |
| CN102049151A (en) * | 2009-10-28 | 2011-05-11 | 中国医学科学院药用植物研究所 | Solid phase extraction column for patulin |
| CN102507805A (en) * | 2011-10-27 | 2012-06-20 | 湖南省产商品质量监督检验院 | Method for detecting trichothecene compound in grain and solid phase extraction column for detection |
Non-Patent Citations (1)
| Title |
|---|
| 滕胜利: ""SXH型三向旋转水冷混合机的机理与应用"", 《第二届高功能涂料的开发与应用技术研讨会》, 30 April 2003 (2003-04-30), pages 202 - 206 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110455943A (en) * | 2019-07-25 | 2019-11-15 | 苏州艾迪迈医疗科技有限公司 | A kind of on-line mixing filler solid-phase extraction column and preparation method thereof |
| CN110455943B (en) * | 2019-07-25 | 2023-04-25 | 重庆大学 | Online mixed filler solid-phase extraction column and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103239889B (en) | 2015-04-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102584918B (en) | Method for preparing high-purity baicalin | |
| CN101864021B (en) | Preparation method of nanometer silicon gel surface gastrodin molecular engram polymers | |
| CN103551131A (en) | Preparation method of polypropylene film micro solid-phase extraction packet based on MIL-101 adsorbent | |
| CN101721979A (en) | Method for preparing macroporous adsorbent resin special for separating valine | |
| CN103482624A (en) | Preparation method for active carbon with photocatalysis function | |
| CN103724394A (en) | Continuous separation purification method of glycyrrhizic acid and glycyrrhiza flavonoids | |
| CN106861236B (en) | A method of utilizing hypercrosslinked polymeric resin adsorbing separation pentanediamine | |
| CN103949204A (en) | Preparation method of multistage pore passage composite molecular sieve adsorbent | |
| CN103239889B (en) | Filling method of small solid-phase extraction column with mixed packing, and small solid-phase extraction column | |
| CN107179367B (en) | Solid phase extraction series column for toxin detection and preparation method thereof | |
| CN102115442B (en) | Method for separating carnosic acid from rosemary leaf extract | |
| CN102060650A (en) | Method for purifying chromatographic grade toluene | |
| CN107014931B (en) | A kind of film modified nano carbon microsphere material of cell and its preparation method and application | |
| CN104498189A (en) | Method for extracting onion oil based on nanometer materials | |
| CN201799135U (en) | Split nano-fiber solid phase extraction column | |
| CN208959374U (en) | A kind of general mixed type solid-phase extraction column | |
| CN109200999B (en) | Preparation method of ion adsorption column applied to polyimide purification | |
| CN1166655C (en) | Process for extracting taxol from filtrate of enqlish yew cell culturing liquid | |
| CN106334344B (en) | Lycorine surface molecule print nanoparticle solid-phase extraction column and its application | |
| CN102516112B (en) | Preparation method for chromatographic grade N,N-dimethyl formamide | |
| CN1298712C (en) | Method for elementary separating 10-noracetyl Baccatins III from branches and leaves of yew | |
| CN107300599A (en) | A kind of method of acidic drug in SPE liquid chromatogram combination examination liquid medicine | |
| CN108033452A (en) | A kind of magnetic mesoporous silica molecule imprinted polymer and its preparation method and application | |
| CN113274978A (en) | Reduced graphene oxide @ zirconium dioxide composite material and application thereof | |
| CN102153437A (en) | Preparation method of organic reagent methyl benzene of high performance liquid chromatography (HPLC) level |
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 | ||
| CP02 | Change in the address of a patent holder |
Address after: 214000 Jiangsu city of Wuxi province Tong Road No. 898 South No. 7 Patentee after: Jiangnan University Address before: No. 1800 road 214122 Jiangsu Lihu Binhu District City of Wuxi Province Patentee before: Jiangnan University |
|
| CP02 | Change in the address of a patent holder |