CN105709458B - A kind of experimental provision that Solid Phase Extraction is carried out to blood sample - Google Patents
A kind of experimental provision that Solid Phase Extraction is carried out to blood sample Download PDFInfo
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- CN105709458B CN105709458B CN201610075636.1A CN201610075636A CN105709458B CN 105709458 B CN105709458 B CN 105709458B CN 201610075636 A CN201610075636 A CN 201610075636A CN 105709458 B CN105709458 B CN 105709458B
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- phase extraction
- solid phase
- solid
- extraction column
- vacuum tank
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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
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- G—PHYSICS
- 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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- G—PHYSICS
- 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
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- 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
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of experimental provisions that Solid Phase Extraction is carried out to blood sample, this experimental provision can make the operation of blood sample Solid Phase Extraction become very convenient, quick, sample pre-treatments speed is greatly accelerated, is improved work efficiency, it is very useful in batch samples pretreatment process.The use of high-penetration flexibility sieve plate, convenient for passing through for macromolecular, also polar molecule can be made easily to wash, convenient for the extraction separation of large scale, legibility in blood sample matrix from sample, effective extraction and separation can be carried out to large-sized substance, and can avoid easily decomposing the dissociation of pharmaceutical preparation, reduce the detection error in metabolic process.
Description
Technical field
The present invention relates to Experiment of Analytical Chemistry pretreatment technology field more particularly to it is a kind of to blood sample carry out solid phase extraction
The experimental provision taken.
Background technology
Solid Phase Extraction（Solid-Phase Extraction, SPE）It is a kind of sorption extraction mistake of absorption-washing-elution
Journey is a kind of sample pretreatment technology, sample can be detached, purified and concentrated.Solid phase is to the adsorption capacity of isolate than molten
The solvent bigger of isolate is solved, the purpose thing rate of recovery is improved compared with liquid-liquid extraction method, it can be more effectively by purpose thing with doing
Disturb object separation.Therefore, solid phase extraction techniques are widely used in the various aspects such as environment measuring analysis, food analysis, Pharmaceutical Analysis.
Certain device is needed in Solid Phase Extraction experimentation to place solid-phase extraction column, container etc., so as to convenient, fast
Complete operation in ground.But in real work, all it is to use carton or the homemade easy device of plank, several pillars can only be placed, and
It is the pillar of single specification, pillar can not be used in series, and can not place associated vessel, and therefore, function is single, and operation is not
Just, working efficiency is low.The extraction of sample and analysis are necessary analyses in pharmacokinetics and metabolism group etc. in blood
Processing method.Due to blood sample matrix complexity, current commercialization solid phase extraction column stuffing is fine and close, it is difficult to large-sized object
Matter (such as liposome) carries out effective extraction and separation.And labile pharmaceutical preparation can also generate different degrees of dissociation, lead
It causes to generate deviation for the detection in metabolic process.In view of the above-mentioned problems, handling this field in blood sample, a kind of energy is provided
The solid phase extraction method of large scale, easy dissociation substance is efficiently separated, is had for the research of some pharmacokinetics very careless
Justice.
Invention content
To overcome more than technical problem, the present invention provides a kind of experimental provisions that Solid Phase Extraction is carried out to blood sample.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of experimental provision that Solid Phase Extraction is carried out to blood sample is extracted including the first solid-phase extraction column, second solid phase
Column and vacuum tank；
First solid-phase extraction column is connect by casing of transferring with second solid phase extraction column, and the switching casing is hollow
Round column tube, the outer wall of the connector of first solid-phase extraction column connect with the inner wall tightening for casing of transferring, the second solid phase
The inner wall of extraction column connects with the outer wall fastening for casing of transferring, and the switching casing and the first solid-phase extraction column and second solid phase extract
Column joint is taken to be equipped with sealing ring；
First solid-phase extraction column（1）With second solid phase extraction column（2）Be be equipped with sieve plate equipped with different fillers
Double-deck solid-phase extraction column, including：Bottom sieve plate（26）, nonpolar silicon substrate filler positioned at bottom（27）, above first layer filler
Fixed screen deck（28）With positioned at fixed screen deck（28）The water imbibition filler of top（29）；The sieve plate is high-penetration flexibility sieve
Plate；
It is fastenedly connected with cover board at the top of the vacuum tank, the side wall at the top of the vacuum tank is equipped with snap-gauge, the lid
It is slidably fixed on the snap-gauge, the junction of the cover board and the vacuum tank is equipped with gasket；On the cover board
It is even to be provided with multiple through-holes, hollow sleeve is inserted in the through-hole, the hollow sleeve is the hollow column tube that gradient is shunk, described
The tip size of hollow sleeve is wider than the through-hole, and the top of the hollow sleeve fastens phase with the second solid phase extraction column
It connects, and connecting pin is located at outside vacuum tank, the outer wall of the connector of the second solid phase extraction column and the inner wall tightening phase of hollow sleeve
It connects, the bottom end of the hollow sleeve is extended in collecting pipe, the hollow sleeve and second solid phase extraction column and through-hole joint
Equipped with sealing ring；
The lower part of the vacuum tank is equipped with the collecting tank alternatively used and hole position plate, the left and right side walls of the vacuum tank
Inside is equipped with guide groove, and the collecting tank and hole position plate are slidably fixed to by guide groove on the side wall of vacuum tank；It is described
The clamping being adapted with guide groove is equipped at left and right sides of collecting tank；A pair at the position of the through-hole is corresponded on the plate of the hole position
It is provided with jack with answering, the collecting pipe is fixed on jack；
The top of guide groove is equipped with bleeding point on the side wall of the vacuum tank, and the bleeding point passes through exhaust tube and vacuum pump
It is connected, vacuum regulator and surge flask is provided on the exhaust tube；Sealing is rotatably connected on the side wall of the vacuum tank
Door；The bottom of the vacuum tank is provided with universal wheel.
Preferably, the universal wheel has 4；
Preferably, it is provided with swing handle on the hermatic door；
Preferably, the side wall of the hermatic door is equipped with gasket；
Preferably, the collecting pipe is test tube, beaker or centrifuge tube；
It is prepared into preferably, the high-penetration flexibility sieve plate is macromolecule filiform non-woven material；
Preferably, the water imbibition packing material size is between 200-300 mesh；
Preferably, the grain size of the nonpolarity silicon substrate filler dry powder is 30-50 μm；
Preferably, the water imbibition filler is calcium oxide, sodium hydroxide, anhydrous magnesium sulfate, solid calcium chloride and solid
One kind in magnesium chloride.
The beneficial effects of the invention are as follows：
A kind of experimental provision that Solid Phase Extraction is carried out to blood sample of the present invention can make the behaviour of blood sample Solid Phase Extraction
Work becomes very convenient, quick, greatly accelerates sample pre-treatments speed, improves work efficiency, is handled before batch samples
It is very useful in the process.Due to the use of hollow sleeve, in pillar and vacuum case lid when can prevent because replacing solid-phase extraction column
Cross contamination occurs for the engaging portion of plate through-hole.The use of switching casing can also realize that the series connection of different size extraction column is used in combination.
Snap-gauge, hole position plate and the slidably design of collecting tank and the design of hermatic door are, it can be achieved that extraction column and collection device replacement side
Just purpose.Suction to different material can be achieved in the use for being equipped with the double-deck solid-phase extraction column equipped with different fillers of sieve plate
Attached, the double-deck solid-phase extraction column equipped with positive sorptive filler and water imbibition filler facilitates moisture impurity removal in organic sample same
Shi Shixian samples cross post separation, enrich the application range of solid-phase extraction column, and adsorbed impurity species increase.High-penetration flexibility is sieved
The use of plate convenient for passing through for macromolecular, can also be such that polar molecule easily washs, convenient for large scale in blood sample matrix, easily
The extraction separation of sample is dissociated, effective extraction and separation can be carried out, and can keep away to large-sized substance (such as liposome)
Exempt from the dissociation of easily decomposition pharmaceutical preparation, reduce the detection error in metabolic process.
Description of the drawings
Fig. 1 is the structure diagram of the embodiment of the present invention.
Fig. 2 is the cross-sectional view of the embodiment of the present invention.
Fig. 3 is the structure diagram of collecting tank of the embodiment of the present invention.
In figure：1:First solid-phase extraction column 2:Second solid phase extraction column 3:Vacuum tank 4:Connector 5：Sealing ring
6：Cover board 7：Snap-gauge 8：Gasket 9：Through-hole 10：Hollow sleeve 11：Collecting pipe 12：Collecting tank 13：Hole position plate 14：It leads
To slot 15：Card adapter plate 16：Jack 17：Hermatic door 18：Bleeding point 19：Exhaust tube 20：Vacuum pump 21：Vacuum regulator
22：Surge flask 23：Universal wheel 24：Swing handle 25：Switching casing 26：Bottom sieve plate 27：Nonpolar silicon substrate filler
28：Fixed screen deck 29：Water imbibition filler.
Specific embodiment
Technical scheme of the present invention is further elaborated with reference to embodiment, and with reference to attached drawing.
As shown in Figure 1, a kind of experimental provision that Solid Phase Extraction is carried out to blood sample, including the first solid-phase extraction column 1, the
Two solid-phase extraction columns 2 and vacuum tank 3；
First solid-phase extraction column 1 is connect by casing 25 of transferring with second solid phase extraction column 2, the switching casing 25
For hollow round column tube, the outer wall of the connector 4 of first solid-phase extraction column 1 connects with the inner wall tightening for casing 25 of transferring, institute
The inner wall for stating second solid phase extraction column 2 connects with the outer wall fastening for casing 25 of transferring, the switching casing 25 and first solid phase extraction
Column 1 and 2 joint of second solid phase extraction column is taken to be equipped with sealing ring 5；
First solid-phase extraction column 1 and second solid phase extraction column 2 are the bilayers equipped with different fillers for being equipped with sieve plate
Solid-phase extraction column, including：Bottom sieve plate 26, the nonpolar silicon substrate filler 27 positioned at bottom, the gravity flow screen above first layer filler
Plate 28 and the water imbibition filler 29 above fixed screen deck 28；The sieve plate is high-penetration flexibility sieve plate；
The top of the vacuum tank 3 is fastenedly connected with cover board 6, and the side wall at 3 top of vacuum tank is equipped with snap-gauge 7, institute
It states cover board 6 to be slidably fixed on the snap-gauge 7, the junction of the cover board 6 and the vacuum tank 3 is equipped with gasket 8；Institute
It states and 3 through-holes 9 is evenly arranged on cover board 6, hollow sleeve 10 is inserted in the through-hole 9, the hollow sleeve 10 is that gradient is received
The hollow column tube of contracting, the tip size of the hollow sleeve 10 are wider than the through-hole 9, the top of the hollow sleeve 10 with it is described
The fastening of second solid phase extraction column 2 connects, and connecting pin is located at outside vacuum tank 3, the connector 4 of the second solid phase extraction column 2
Outer wall connects with the inner wall tightening of hollow sleeve 10, and the bottom end of the hollow sleeve 10 is extended in collecting pipe 11, described hollow
Casing 10 is equipped with sealing ring 5 with second solid phase extraction column 2 and 9 joint of through-hole；
The lower part of the vacuum tank 3 is equipped with the collecting tank 12 that alternatively uses and hole position plate 13, a left side for the vacuum tank 3,
Guide groove 14 is equipped on the inside of right side wall, the collecting tank 12 and hole position plate 13 are slidably fixed to vacuum tank by guide groove 14
On 3 side wall；12 left and right sides of collecting tank is equipped with the card adapter plate 15 being adapted with guide groove 14；It is right on the plate 13 of the hole position
It answers and is provided with 3 jacks 16 at the position of the through-hole 9 correspondingly, the collecting pipe 11 is fixed on jack 16；It is described
The top of guide groove 14 is equipped with bleeding point 18 on the side wall of vacuum tank 3, and the bleeding point 18 passes through exhaust tube 19 and vacuum pump 20
It is connected, vacuum regulator 21 and surge flask 22 is provided on the exhaust tube 19；It is rotatablely connected on the side wall of the vacuum tank 3
There is hermatic door 17, state and swing handle is provided on hermatic door, the side wall of the hermatic door is equipped with gasket；The vacuum tank 3
Bottom be provided with universal wheel 23, it is preferred that the universal wheel has 4；The collecting pipe can be test tube, beaker or centrifugation
Pipe；Preferably, the high-penetration flexibility sieve plate is that macromolecule filiform non-woven material is prepared into, the water imbibition filler grain
Diameter is between 200-300 mesh；Preferably, the grain size of the nonpolar silicon substrate filler dry powder is 30-50 μm；The water imbibition is filled out
Expect for one kind in calcium oxide, sodium hydroxide, anhydrous magnesium sulfate, solid calcium chloride and solid magnesium chloride.
Claims (5)
1. a kind of experimental provision that Solid Phase Extraction is carried out to blood sample, it is characterised in that：Including the first solid-phase extraction column（1）、
Second solid phase extraction column（2）And vacuum tank（3）；
First solid-phase extraction column（1）Pass through casing of transferring（25）With second solid phase extraction column（2）Connection, the switching casing
（25）For hollow round column tube, first solid-phase extraction column（1）Connector（4）Outer wall with switching casing（25）Inner wall it is tight
Solid phase connects, the second solid phase extraction column（2）Inner wall with switching casing（25）Outer wall fastening connect, the switching casing
（25）With the first solid-phase extraction column（1）With second solid phase extraction column（2）Joint is equipped with sealing ring（5）；
First solid-phase extraction column（1）With second solid phase extraction column（2）It is the bilayer equipped with different fillers for being equipped with sieve plate
Solid-phase extraction column, including：Bottom sieve plate（26）, nonpolar silicon substrate filler positioned at bottom（27）, fixed screen deck above filler
（28）With positioned at fixed screen deck（28）The water imbibition filler of top（29）；The sieve plate is high-penetration flexibility sieve plate；
The vacuum tank（3）Top be fastenedly connected with cover board（6）, the vacuum tank（3）The side wall at top is equipped with snap-gauge
（7）, the cover board（6）It is slidably fixed to the snap-gauge（7）On, the cover board（6）With the vacuum tank（3）Junction
Equipped with gasket（8）；The cover board（6）On be evenly arranged with multiple through-holes（9）, the through-hole（9）Inside it is inserted with hollow sleeve
（10）, the hollow sleeve（10）Be gradient shrink hollow column tube, the hollow sleeve（10）Tip size be wider than it is described
Through-hole（9）, the hollow sleeve（10）Top and the second solid phase extraction column（2）Fastening connects, and connecting pin is located at very
Empty van（3）Outside, the second solid phase extraction column（2）Connector（4）Outer wall and hollow sleeve（10）Inner wall tightening connect,
The hollow sleeve（10）Bottom end extend to collecting pipe（11）It is interior, the hollow sleeve（10）With second solid phase extraction column（2）
And through-hole（9）Joint is equipped with sealing ring（5）；
The vacuum tank（3）Lower part be equipped with the collecting tank that alternatively uses（12）With hole position plate（13）, the vacuum tank（3）'s
Guide groove is equipped on the inside of left and right side walls（14）, the collecting tank（12）With hole position plate（13）Pass through guide groove（14）Slideably
It is fixed on vacuum tank（3）Side wall on；The collecting tank（12）The left and right sides is equipped with and guide groove（14）The card adapter plate being adapted
（15）；Hole position plate（13）The upper correspondence through-hole（9）Position at be provided with jack correspondingly（16）, the collection
Pipe（11）It is fixed on jack（16）On；
The vacuum tank（3）Side wall on guide groove（14）Top be equipped with bleeding point（18）, the bleeding point（18）Pass through pumping
Tracheae（19）With vacuum pump（20）It is connected, the exhaust tube（19）On be provided with vacuum regulator（21）And surge flask（22）；
The vacuum tank（3）Side wall on be rotatably connected to hermatic door（17）；The vacuum tank（3）Bottom be provided with universal wheel
（23）；
The high-penetration flexibility sieve plate is that macromolecule filiform non-woven material is prepared into, and the water imbibition packing material size exists
Between 200-300 mesh, the grain size of the nonpolarity silicon substrate filler dry powder is 30-50 μm；The water imbibition filler for calcium oxide,
One kind in sodium hydroxide, anhydrous magnesium sulfate, solid calcium chloride and solid magnesium chloride.
2. a kind of experimental provision that Solid Phase Extraction is carried out to blood sample as described in claim 1, it is characterised in that：Described ten thousand
To wheel（23）There are 4.
3. a kind of experimental provision that Solid Phase Extraction is carried out to blood sample as described in claim 1, it is characterised in that：It is described close
Closure door（17）On be provided with swing handle（24）.
4. a kind of experimental provision that Solid Phase Extraction is carried out to blood sample as described in claim 1, it is characterised in that：It is described close
Closure door（17）Side wall be equipped with gasket.
5. a kind of experimental provision that Solid Phase Extraction is carried out to blood sample as described in claim 1, it is characterised in that：The receipts
Collector（11）It is test tube, beaker or centrifuge tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610075636.1A CN105709458B (en) | 2016-02-03 | 2016-02-03 | A kind of experimental provision that Solid Phase Extraction is carried out to blood sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610075636.1A CN105709458B (en) | 2016-02-03 | 2016-02-03 | A kind of experimental provision that Solid Phase Extraction is carried out to blood sample |
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| CN105709458A CN105709458A (en) | 2016-06-29 |
| CN105709458B true CN105709458B (en) | 2018-06-29 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105641971B (en) * | 2016-03-21 | 2018-05-01 | 河南师范大学 | A kind of comprehensive solid-phase extraction device |
| CN108225883B (en) * | 2016-12-09 | 2020-04-17 | 中国科学院大连化学物理研究所 | Solid phase extraction and blowing integrated device and use method |
| CN107748099B (en) * | 2017-10-20 | 2020-09-01 | 西北大学 | Preparation method of self-heating solid-phase saponification extraction column for pretreatment of blood sample |
| CN109100203A (en) * | 2018-08-22 | 2018-12-28 | 佛山科学技术学院 | A kind of solid-phase extraction column for residue of veterinary drug measurement |
| CN109163951B (en) * | 2018-11-05 | 2021-09-07 | 长沙都正医学检验有限责任公司 | Preparation facilities of TMAO negative sample |
| CN114034537A (en) * | 2021-09-16 | 2022-02-11 | 拉萨海关技术中心 | Solid phase extraction equipment for food detection and separation method |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE29910726U1 (en) * | 1998-06-12 | 1999-09-02 | Analyticon Ag Biotechnologie P | Device for the liquid-chromatographic separation of mixtures of substances under pressure |
| CN201454152U (en) * | 2009-07-07 | 2010-05-12 | 上海新拓分析仪器科技有限公司 | Positive-pressure solid-phase extracting device |
| CN102841148A (en) * | 2011-06-20 | 2012-12-26 | 苏州赛分科技有限公司 | Switch cannula for solid- phase extraction column |
| CN103575829A (en) * | 2012-07-24 | 2014-02-12 | 天津市圣信唯科技有限公司 | A solid-phase extraction device |
| CN104248862B (en) * | 2014-09-18 | 2016-01-06 | 李清 | A kind of experimental provision sample extracting solution being carried out to SPE |
| CN104606923B (en) * | 2015-01-16 | 2016-06-29 | 北京大学 | A kind of flexible sieve plate solid-phase extraction column and its preparation method and application |
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