CN108152429A - A kind of Solid Phase Extraction microtrabeculae and application - Google Patents
A kind of Solid Phase Extraction microtrabeculae and application Download PDFInfo
- Publication number
- CN108152429A CN108152429A CN201611098737.7A CN201611098737A CN108152429A CN 108152429 A CN108152429 A CN 108152429A CN 201611098737 A CN201611098737 A CN 201611098737A CN 108152429 A CN108152429 A CN 108152429A
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- solid phase
- phase extraction
- diameter
- cylinder
- microtrabeculae
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a kind of Solid Phase Extraction microtrabeculae, which is made of cylinder, sieve plate and filler.Two end faces of the extraction microtrabeculae can compression seal, suitable for Full-automatic solid phase extraction device, enrichment method purification pre-treatment can be carried out to fluid sample, is analyzed for the separation of follow-up high performance liquid chromatography.
Description
Technical field
The invention belongs to analytical chemistry field, more particularly to a kind of Solid Phase Extraction microtrabeculae for sample pre-treatments.It should
Extraction column is a kind of novel Solid Phase Extraction microtrabeculae.Full-automatic solid phase extraction device can be coordinated, be suitble to the automatic solid of fluid sample
Mutually extraction pre-treatment.
Background technology
Solid Phase Extraction (Solid Phase Extraction, abbreviation SPE) is grown up since the eighties mid-term
A Sample Pretreatment Technique.It is combined and developed by liquid-solid extraction and liquid chromatography technology.It is mainly used for point of sample
From purification and enrichment.Main purpose is to reduce sample substrate interference, raising detection sensitivity.SPE technologies are based on liquid-solid phase
Chromatographic theory is enriched with sample by the way of selective absorption, selective elution, is detached, is purified, and is that one kind includes liquid
The physical extraction process of phase and solid phase；It can also approx be regarded as to a kind of simple chromatographic process.SPE is to utilize selectivity
Absorption and the liquid chromatography separation principle of selective elution.More common method is that fluid sample solution is made to pass through adsorbent,
Retain wherein measured matter, then appropriate strength solvents is selected to wash away impurity, then elute measured matter rapidly with a small amount of solvent, from
And achieve the purpose that quick separating purification and concentration.Also alternative adsorptive hindrance impurity, and measured matter is allowed to flow out；Or simultaneously
Adsorbing contaminant and measured matter reuse suitable solvent selectivity elution measured matter.Traditional SPE approach process take compared with
Long, the mode of generally use static pressure carries out loading, cleaning and elution.It is cumbersome since manually time-consuming for SPE processes,
Part apparatus manufacture is proposed automatic SPE devices.Automatic SPE be it is a set of by liquid handling platform derivative develop can be in nothing
The solid-phase extracting instrument of automatic operating solid phase extraction method in the case of people is on duty.Generally comprise the activation of solid-phase extraction column, loading,
Cleaning, elution and the switching of sample and etc..The prior art is divided into single channel solid-phase extracting instrument and Multi-channel solid phase extraction instrument.
Most automatic SPE equipment also has the process that nitrogen blows concentration, to improve chromatography column feed materials concentration after elution.These automatic SPE dresses
Although putting realizes automation, treated, and sample can not be directly entered chromatographic system, still need to manually shift.Holland
A multichannel automatic solid-phase extractor that SPARK companies release, realizes the combination of full-automatic SPE and chromatography.With in the market
The difference of other products is：Target substance of the extracting and enriching on solid-phase extraction column elutes and is directly entered chromatography under high pressure
Column carries out separation analysis, eliminates the step of eluent is collected, nitrogen blows concentration and constant volume, improves the sample rate of transform and repetition
Property.But the product is first captured solid-phase extraction column by manipulator to loading position, is then captured by the way of robotic arm manipulation
The extraction column is transferred to elution sample introduction position.This mode seals every time there are the compression sealing orientation problem of solid-phase extraction column
Impression does not repeat, and the reusable number of reality for leading to solid-phase extraction column is 3 times.And the apparatus structure is complicated, price is held high
It is expensive.Full-automatic solid phase extraction device (the Chinese patent that Dalian Inst of Chemicophysics, Chinese Academy of Sciences proposes
201510920927.1) solid-phase extraction column is placed using array disk, accurately pallet is controlled to rotate using stepper motor, avoided
Manipulator repeatedly captures the step of positioning, simplifies process, improves reliability, with the extraction microtrabeculae of the present invention, can repeat
It uses 10 times.The Solid Phase Extraction microtrabeculae of the present invention is designed for cooperation Full-automatic solid phase extraction device, and both ends are resistant to
The sealing of 20MPa pressure, while be also equipped with being easy to autoregistration, reliability is high, with ensure be not in use leakage,
Phenomena such as filler caves in prolongs the service life.
Invention content
The object of the present invention is to provide a kind of Solid Phase Extraction microtrabeculaes, and both ends is suitble to compress the mode of sealing, and cooperation is cut automatically
It changes valve and carries out flow path switching, realize Full-automatic solid phase extraction process.The extraction column can coordinate Full-automatic solid phase extraction device, and
It can repeatedly regenerate and reuse.
The technical scheme is that：
A kind of Solid Phase Extraction microtrabeculae, is made of cylinder, sieve plate and filler；The cylinder is cylinder, two above and below cylinder
End offers the circular groove of the axis centered on column axis, and axle center opens up that there are one through the axial round of two groove floors
Through-hole, groove makes the upper and lower ends of the through-hole form stepped hole, for fixed screen deck；Two fixed screen decks are respectively placed in the platform to be formed
In rank hole；The diameter of sieve plate is more than step bore dia, and the step bore dia of fixed screen deck is more than the diameter of through-hole；The filler is tight
In the close through-hole being filled between two fixed screen decks；The ratio between outer diameter and diameter of bore of the cylinder are 6:1~3:1；Described
At 1/2 height of cylinder outer wall, radially equipped with an annular groove, it is automatically positioned for coordinating.
The outer diameter of the cylinder is 6~16 millimeters, and diameter of bore is 1~4 millimeter, and a length of 8~16 millimeters, column both ends are close
Cover, material used are high molecular material.The high molecular material is Kynoar, nylon or composite material.
The sieve plate is stainless steel sieve, and diameter is bigger 0.1mm than the step aperture of fixed screen deck, 0.8~1.2mm of thickness, sieve
3~7 microns of panel aperture is smaller than the particle diameter of filler by more than 30%.
The filler is phase chromatography-use filler, surface bond polarity or non-polar group, for the target of opposed polarity
Component extracting；A diameter of 5~20 microns of filler particles.
The preparation method of the solid phase microextraction column comprises the steps of：Cylinder prepares：By precision machinery processing or
It moulds molding mode, prepares Solid Phase Extraction cylinder, it is spare after cleaning-drying；Filling：Stainless steel sieve is embedded in cylinder one end, by
Other end opening inserts appropriate filler, and continuous shaking cylinder, makes filler closely tamp during inserting.After the full filler of filling,
Stainless steel sieve is embedded in the other end and is compressed.
The application method of the solid-phase extraction column：
The solid phase microextraction column is placed in the through-hole on the array disk of Full-automatic solid phase extraction device, using logical
The cooperation slotted in the middle part of the positioning O circles of hole inner wall insertion and extraction cylinder is centered about.The Full-automatic solid phase extraction dress
It puts according to the time sequential routine, carries out Solid Phase Extraction microtrabeculae successively and compress sealing, sample loading, elution, then automatic displacement, compresses close
Envelope and high pressure elution the step of, complete target analysis component enrichment method and elution sample introduction, target components enter chromatographic column into
Row separation analysis.
Compared with conventional solid extraction column, both ends can pressurize liquid the Solid Phase Extraction microtrabeculae of the present invention, be suitable for
Full-automatic solid phase extraction device；And the not reversible pressurization of conventional solid extraction column, it is not used to Full-automatic solid phase extraction device.This
Invention makes cylinder using high molecular materials such as Kynoar, nylon, by control pressure and sealed knife mouth-shaped, realizes anti-
Multiple pressure-resistant seal improves the service life and reliability of Solid Phase Extraction microtrabeculae.
Description of the drawings
Fig. 1 is Solid Phase Extraction microtrabeculae schematic diagram.Wherein, 1 --- cylinder, 2 --- sieve plate, 3 --- filler, 4 --- annular
Groove
1 chromatogram of Fig. 2 application examples.5-a is tea extract chromatogram.5-b mixes mark chromatogram for polycyclic aromatic hydrocarbon.5-c is
Tea extract adds cycloaromatics and mixes mark chromatogram.1- naphthalenes, 2- acenaphthenes, 3- is luxuriant and rich with fragrance, 4- fluoranthene, 5- pyrenes.
Specific embodiment
Illustrate the present invention, but do not form limitation of the invention below by embodiment.
Embodiment 1
A kind of Solid Phase Extraction microtrabeculae, as shown in Figure 1, being made of cylinder 1, sieve plate 2 and filler 3.Its middle column body 1 is outer diameter
The cylinder of 9mm, internal diameter 2.2mm.The upper and lower end face of 1 endoporus of cylinder offers 2.4 millimeters of diameter, sieve plate 1.2 millimeters deep is consolidated
Determine stepped hole；Sieve plate 2 be outer diameter 2.5mm, thickness 1mm, the stainless steel sieve that 3 microns of aperture, mounted on sieve plate fix stepped hole
It is interior.Filler 3 is the C18 modified silica-gel fillers of 10 microns of grain size, in the tightly packed hole between two sieve plates.The length of cylinder 1
It is 10 millimeters.1 outer wall upper edge of cylinder is radially provided with an annular groove 4, and 1.2 millimeters of well width is 0.5 millimeter deep, in cylinder 1
Between position.The material of cylinder 1 is Kynoar.
Application examples 1：
The Solid Phase Extraction microtrabeculae finished will be prepared, be placed in the disk through-hole on Full-automatic solid phase extraction device, utilized
Automatic centering positioning is realized in the cooperation slotted in the middle part of the positioning O circles of through-hole wall insertion and extraction cylinder.According to full-automatic solid phase
The time sequential routine of extraction equipment carries out compression sealing, sample loading, elution, high pressure elution and liquid-phase chromatographic column loading successively
Step, the enrichment method of target analysis component and elution sample introduction, target components enter chromatographic column and are detached in complete paired samples
Analysis.Pre-treatment is carried out to Tea Samples using microtrabeculae described in embodiment 1, step is as follows：
Prepare tea extract：1g tealeaves adds 5 ml methanol ultrasounds after ten minutes, sealing and standing 24 hours, filters tea
Leaf extract, constant volume are diluted to 200mL.
Prepare mark-on tea extract：1g tealeaves, after ten minutes, sealing and standing 24 hours filters tea to 5 ml methanol ultrasounds
Leaf extract adds in polycyclic aromatic hydrocarbon and mixes mark mother liquor, and constant volume is diluted to 200mL, a concentration of 1ppm of polycyclic aromatic hydrocarbon.
It draws 200 microlitres of samples successively on autosampler, injects solid-phase extraction column.Cleaning solution is pumped into, cleans solid phase
Extraction column.After completing cleaning, solid-phase extraction column pallet rotates one, and solid-phase extraction column turns to elution sample position, and six-way valve rotates,
Target components in solid-phase extraction column under the action of liquid chromatogram mobile phase, are directly eluted into chromatographic column and carry out separation point
Analysis.Analysis of spectra is shown in Fig. 2.
Claims (6)
1. a kind of Solid Phase Extraction microtrabeculae, it is characterised in that：It is made of cylinder (1), sieve plate (2) and filler (3)；The cylinder (1)
For cylinder, the circular groove of the axis centered on column axis is offered in cylinder upper and lower ends, axle center opens up that there are one pass through
Wear the axial circular through hole of two groove floors, groove makes the upper and lower ends of the through-hole form stepped hole, for fixed screen deck (2),
Two fixed screen decks (2) are respectively placed in the stepped hole to be formed；The diameter of sieve plate is more than step bore dia, the stepped hole of fixed screen deck
Diameter is more than the diameter of through-hole；In the tightly packed through-hole between two fixed screen decks of the filler (3)；The cylinder (1)
The ratio between outer diameter and diameter of bore are 6:1~3:1；It is radially recessed equipped with an annular at 1/2 height of the cylinder (1) outer wall
Slot (4) is automatically positioned for coordinating.
2. Solid Phase Extraction microtrabeculae according to claim 1, it is characterised in that：The outer diameter of the cylinder (1) is 6~16 millis
Rice, diameter of bore are 1~4 millimeter, and a length of 8~16 millimeters, column both ends are sealing surface, and material used is high molecular material.
3. Solid Phase Extraction microtrabeculae according to claim 2, it is characterised in that：The high molecular material for Kynoar,
Nylon or composite material.
4. Solid Phase Extraction microtrabeculae according to claim 1, it is characterised in that：The sieve plate be stainless steel sieve, diameter ratio
The big 0.1mm in step aperture of fixed screen deck, 0.8~1.2mm of thickness, 3~7 microns of hole diameter of sieve (perforated) plate, the particle diameter than filler (3) are small
More than 30%.
5. Solid Phase Extraction microtrabeculae according to claim 1, it is characterised in that：The filler be phase chromatography-use filler, table
Face is bonded polarity or non-polar group, is extracted for the target components of opposed polarity；A diameter of 5~20 microns of filler particles.
6. a kind of application of any Solid Phase Extraction microtrabeculaes of claim 1-5 in Solid Phase Extraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611098737.7A CN108152429A (en) | 2016-12-04 | 2016-12-04 | A kind of Solid Phase Extraction microtrabeculae and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611098737.7A CN108152429A (en) | 2016-12-04 | 2016-12-04 | A kind of Solid Phase Extraction microtrabeculae and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108152429A true CN108152429A (en) | 2018-06-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611098737.7A Pending CN108152429A (en) | 2016-12-04 | 2016-12-04 | A kind of Solid Phase Extraction microtrabeculae and application |
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| CN (1) | CN108152429A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724623A (en) * | 2019-09-10 | 2020-01-24 | 深圳市百迈生命科学有限公司 | 1536 well solid phase synthesis and extraction plate |
| CN112915589A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Filler filling device of solid-phase extraction column and application thereof |
| CN115078615A (en) * | 2022-08-22 | 2022-09-20 | 湖南德米特仪器有限公司 | Extraction column for liquid chromatography |
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| EP2278325A1 (en) * | 2009-07-13 | 2011-01-26 | Spark Holland B.V. | Flow through cartridge for selecting an analyte online with high performance liquid chromatography |
| CN102301218A (en) * | 2009-01-29 | 2011-12-28 | 株式会社日立高新技术 | Device for pretreating sample and mass spectrometer equipped with same |
| CN202141701U (en) * | 2011-06-20 | 2012-02-08 | 苏州赛分科技有限公司 | Small column for solid phase extraction processing |
| CN203564815U (en) * | 2013-11-25 | 2014-04-30 | 河南科技学院 | Centrifugal solid-phase extraction column |
| CN203750217U (en) * | 2014-04-01 | 2014-08-06 | 北京润东仪器厂 | Automatic solid-phase extraction equipment |
| CN105466905A (en) * | 2015-10-27 | 2016-04-06 | 厦门市普识纳米科技有限公司 | Solid phase extraction column integrated surface enhanced Raman detection chip |
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2016
- 2016-12-04 CN CN201611098737.7A patent/CN108152429A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102301218A (en) * | 2009-01-29 | 2011-12-28 | 株式会社日立高新技术 | Device for pretreating sample and mass spectrometer equipped with same |
| EP2278325A1 (en) * | 2009-07-13 | 2011-01-26 | Spark Holland B.V. | Flow through cartridge for selecting an analyte online with high performance liquid chromatography |
| CN202141701U (en) * | 2011-06-20 | 2012-02-08 | 苏州赛分科技有限公司 | Small column for solid phase extraction processing |
| CN203564815U (en) * | 2013-11-25 | 2014-04-30 | 河南科技学院 | Centrifugal solid-phase extraction column |
| CN203750217U (en) * | 2014-04-01 | 2014-08-06 | 北京润东仪器厂 | Automatic solid-phase extraction equipment |
| CN105466905A (en) * | 2015-10-27 | 2016-04-06 | 厦门市普识纳米科技有限公司 | Solid phase extraction column integrated surface enhanced Raman detection chip |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724623A (en) * | 2019-09-10 | 2020-01-24 | 深圳市百迈生命科学有限公司 | 1536 well solid phase synthesis and extraction plate |
| CN112915589A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Filler filling device of solid-phase extraction column and application thereof |
| CN115078615A (en) * | 2022-08-22 | 2022-09-20 | 湖南德米特仪器有限公司 | Extraction column for liquid chromatography |
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Application publication date: 20180612 |
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