CN108956258A - Solid-phase extracting disk and its processing method for bulk sample - Google Patents
Solid-phase extracting disk and its processing method for bulk sample Download PDFInfo
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- CN108956258A CN108956258A CN201710363877.0A CN201710363877A CN108956258A CN 108956258 A CN108956258 A CN 108956258A CN 201710363877 A CN201710363877 A CN 201710363877A CN 108956258 A CN108956258 A CN 108956258A
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- 239000007790 solid phase Substances 0.000 title claims abstract description 51
- 238000003672 processing method Methods 0.000 title claims abstract description 16
- 238000000605 extraction Methods 0.000 claims abstract description 32
- 239000000284 extract Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims description 32
- 239000000945 filler Substances 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000003480 eluent Substances 0.000 claims description 4
- 125000000524 functional group Chemical group 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims 3
- 239000007787 solid Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 12
- 239000000523 sample Substances 0.000 description 46
- 238000013461 design Methods 0.000 description 11
- 239000000049 pigment Substances 0.000 description 10
- 238000005070 sampling Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000012856 packing Methods 0.000 description 5
- 239000013618 particulate matter Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 239000004098 Tetracycline Substances 0.000 description 3
- 239000008364 bulk solution Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229960002180 tetracycline Drugs 0.000 description 3
- 235000019364 tetracycline Nutrition 0.000 description 3
- 229930101283 tetracycline Natural products 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 241000036318 Callitris preissii Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- KIPLYOUQVMMOHB-MXWBXKMOSA-L [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O Chemical compound [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O KIPLYOUQVMMOHB-MXWBXKMOSA-L 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- CYDMQBQPVICBEU-UHFFFAOYSA-N chlorotetracycline Natural products C1=CC(Cl)=C2C(O)(C)C3CC4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-UHFFFAOYSA-N 0.000 description 1
- 229960004475 chlortetracycline Drugs 0.000 description 1
- CYDMQBQPVICBEU-XRNKAMNCSA-N chlortetracycline Chemical compound C1=CC(Cl)=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-XRNKAMNCSA-N 0.000 description 1
- 235000019365 chlortetracycline Nutrition 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000000769 gas chromatography-flame ionisation detection Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229940063650 terramycin Drugs 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
Classifications
-
- 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
- G01N1/4005—Concentrating samples by transferring a selected component through a membrane
-
- 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
Abstract
The invention discloses a kind of solid-phase extracting disks and its processing method for bulk sample, the solid-phase extracting disk includes solid-phase extracting disk, including the shell being made of upper cover and chassis, the upper cover and chassis are bonded together by ultrasonic sealing, extract layer is equipped between the upper cover and chassis, filtering/supporting layer is provided between the extract layer and upper cover, chassis, the outer surface on the upper cover and chassis is provided through standard Luer mouth, and the inner surface on the upper cover and chassis is provided with liquid flow path；The liquid flow path is symmetrical along the radial direction of disc face, and the length of the liquid flow path is 10-25mm, and 15 ° -45 ° of angle is formed between two neighboring liquid flow path.Provided by the present invention for the solid-phase extracting disk and its processing method of bulk sample, the existing higher rate of recovery and stability, and the uniformity of extraction can be improved, dead volume is reduced, and can facilitate and realize various general connections, greatly promotes the convenience used.
Description
Technical field
The present invention relates to a kind of solid-phase extracting disk and its processing method more particularly to a kind of solid phases for bulk sample
Extracting disk and its processing method.
Background technique
Bulk sample, such as environmental water sample, the poisonous and harmful substance containing trace.It is conventional because content is very low
Analysis instrument cannot reach the sensitivity of direct injection analysis, need to carry out the sample of large volume the enrichment of trace materials.Than
More typical method is to carry out Solid Phase Extraction, especially suitable for bulk sample processing, referred to as Solid Phase Extraction in Solid Phase Extraction
Disk or Solid Phase Extraction diaphragm.Because the volume of sample is excessive, it is necessary to carry out special designing ability for the structure of Solid Phase Extraction
Meet the requirement of Rapid Extraction.In the market existing product be most importantly 3M company Empore Solid Phase Extraction diaphragm and
The Speedisk solid-phase extracting disk of J.T.Baker company.
The Empore Solid Phase Extraction diaphragm of 3M company, which needs to be equipped with individual equipment or device, to be used, and product is from knot
It can not be connect with general interface on structure, therefore also be not used to the connection of Full-automatic solid phase extraction instrument, when going out to sample
Need to carry special negative pressure extraction device, the sample cup volumes of the device only have 1L, cannot achieve continuous bulk sample
Processing, the Solid Phase Extraction diaphragm structure of 3M are as shown in Figure 1；Fig. 1 comes from american documentation literature US6492183, including monolithic multilayer
Spe membrane 10, the first porous support layer 12, the second porous support layer 14, the boundary 16 of spe membrane, solid phase extraction medium layer 18 are fine
Wiki matter 20 and absorbent particles 22.The Speedisk solid-phase extracting disk of J.T.Baker company has same problem, because it is tied
Structure design is only applicable to negative pressure mode, and the upper end of extracting disk is fixed sample cell, although extracting disk lower end can with Rule mouth
It is connect with facilitating with manually solid-phase extraction device, but cannot achieve the combination with Full-automatic solid phase extraction instrument, it also can not be real
It is now connect with the peristaltic pump of bulk solutions sampling apparatus, Speedisk Solid Phase Extraction dish structure is as shown in Fig. 2, include lower bottom base
10 ', support screen 15 fills the SPE extracting disk 20 ' of full adsorbent, sample cell 25 and fixture 30.
Therefore both above-mentioned products have respective drawback.It is therefore desirable to carry out to existing solid-phase extracting disk
It improves, can be realized the connection of zero obstacle, easily connect bulk sampling pipe, various Solid Phase Extraction hand gears, full-automatic solid phase
Extraction equipment and bulk solutions sampling apparatus.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of solid-phase extracting disk for bulk sample and its processing
Method, the existing higher rate of recovery and stability, and the uniformity of extraction can be improved, dead volume is reduced, and realization can be facilitated each
The general connection of kind, greatly promotes the convenience used.
The present invention is to solve above-mentioned technical problem and the technical solution adopted is that provide a kind of consolidating for bulk sample
Phase extracting disk, including the shell being made of upper cover and chassis, wherein the upper cover and chassis are bonded in one by ultrasonic sealing
It rises, extract layer is equipped between the upper cover and chassis, filtering/supporting layer is provided between the extract layer and upper cover, chassis,
The outer surface on the upper cover and chassis is provided through standard Luer mouth, and the inner surface on the upper cover and chassis is provided with liquid flow
Road.
The above-mentioned solid-phase extracting disk for bulk sample, wherein the inner surface on the upper cover and chassis is disc face,
The liquid flow path is symmetrical along the radial direction of disc face, and the length of the liquid flow path is 10-25mm, two neighboring liquid
15 ° -45 ° of angle is formed between body flow path.
The above-mentioned solid-phase extracting disk for bulk sample, wherein be also formed with annular on the inner surface on the chassis
Slot, the annular groove are connected with radially-arranged liquid flow path.
The above-mentioned solid-phase extracting disk for bulk sample, wherein the upper cover and the material on chassis are polypropylene.
The above-mentioned solid-phase extracting disk for bulk sample, wherein the filtering/supporting layer material is micron-sized PP
Filter membrane or glass fiber filter.
The above-mentioned solid-phase extracting disk for bulk sample, wherein the extraction stuffing in the extract layer is a variety of officials
The silica filler or polymer filler that can be rolled into a ball, the partial size of the extraction stuffing are 10um-100um, the extraction stuffing upper and lower two
The filter disc that thickness is less than 0.5mm is placed in face, and the extraction stuffing suppresses the lamellar structure for forming 3-5mm together with upper and lower filter disc.
The present invention also provides a kind of Solid Phase Extraction processing method of bulk sample to solve above-mentioned technical problem, in use
The solid-phase extracting disk for bulk sample stated includes the following steps: a) to select HLB or PSD as the extraction in extract layer
Filler；B) 5-10L sample is obtained, after activator and poising agent mixing is added, from upper cover Rule mouth with 25mL/min-75mL/min
Flow control mixed liquor enter solid-phase extracting disk；C) after the completion of extracting, eluant, eluent cleaning is added.
The Solid Phase Extraction processing method of above-mentioned bulk sample, wherein the conduct of 15-30ml methanol is added in the step b)
15-30ml deionized water is added as poising agent in activator, and 15-30ml methanol or 20-40ml dichloro is added in the step c)
Methane is as eluant, eluent.
The Solid Phase Extraction processing method of above-mentioned bulk sample, wherein further include by the chassis of multiple solid-phase extracting disks
It is connected in series with upper cover.
The Solid Phase Extraction processing method of above-mentioned bulk sample, wherein the extraction stuffing in the extract layer is a variety of
The silica filler or polymer filler of functional group, the partial size of the extraction stuffing are 10um-100um, the multiple series connection solid phase
The partial size of the extraction stuffing of extracting disk successively becomes smaller.
The present invention, which compares the prior art, to be had following the utility model has the advantages that the solid phase provided by the present invention for bulk sample extracts
Take disk and its processing method, by solid-phase extracting disk use sonic bonding techniques, seamless welding, especially with bulk solutions
When the connection of sampling apparatus, as sample volume increases, subtle particulate matter can constantly be gathered in the filtering of extracting disk in sample
Layer, the pressure for causing extracting disk to be born is increasing, and compared with hickey, the welding manner of ultrasonic bonds can be by sample
The probability revealed because pressure is excessive is preferably minimized.The liquid flow path design inside extracting disk can guarantee that sample uniformly divides simultaneously
Cloth can minimize dead volume in extracting disk.It is tested by consumption pigment, in 25mL/min-75mL/min
Any experimental flow rate under, from the outside observation it can be seen that pigment be evenly distributed in extracting disk, destroy extracting disk by force, send out
Existing pigment is strictly uniform in the distribution of extracting disk packing layer.The test of consumption pigment is carried out again, then uses organic solvent
Elution drains and destroys extracting disk after eluting solvent by force, discovery pigment not in any margin residual of extracting disk packing layer,
Illustrate the flow path designs of extracting disk can fully ensure that extracting disk uniformity and the smallest dead volume.
Detailed description of the invention
Fig. 1 is the Empore Solid Phase Extraction diaphragm structure schematic diagram of existing 3M company；
Fig. 2 is the Speedisk solid-phase extracting disk structural schematic diagram of existing J.T.Baker company；
Fig. 3 is the solid-phase extracting disk decomposition texture schematic diagram that the present invention is used for bulk sample；
Fig. 4 is the solid-phase extracting disk the schematic diagram of the section structure that the present invention is used for bulk sample；
Fig. 5 is the liquid flow path distribution schematic diagram of solid-phase extracting disk of the present invention.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 3 is the solid-phase extracting disk decomposition texture schematic diagram that the present invention is used for bulk sample；Fig. 4 is the present invention for big
The solid-phase extracting disk the schematic diagram of the section structure of volume sample.
Fig. 3 and Fig. 4 are referred to, provided by the present invention for the solid-phase extracting disk of bulk sample, shell is by upper cover 1 and bottom
2 two parts of disk composition.Upper cover 1 and the material on chassis 2 are polypropylene, are applied to needed for being resistant in Solid Phase Extraction various
Eluting solvent.Upper cover 1 and chassis 2 are sealed using the technology of ultrasonic bonds, the intensity of welding close to one piece of entirety PP material,
It can be resistant to the pressure of 100pci, compared with hickey, the sealing means of ultrasonic bonds can be excessive because of pressure by sample
And the probability revealed is preferably minimized.Upper cover 1 and chassis 2 have carried out the design of symmetry liquid flow path, the length of liquid flow path respectively
The angle spent between 10-25mm etc., liquid flow path differs between 15-45 °, to guarantee the uniform of sample solution distribution
Property.It is tested by consumption pigment, under any experimental flow rate of 25mL/min-75mL/min, observation be can see from the outside
Pigment is evenly distributed in extracting disk, destroys extracting disk by force, and discovery pigment is strictly equal in the distribution of extracting disk packing layer
Even.The test of consumption pigment is carried out again, is then eluted with solvent, is drained eluting solvent and is destroyed extracting disk by force later, sends out
Existing pigment illustrates that the flow path designs of extracting disk can fully ensure that extracting disk not in any margin residual of extracting disk packing layer
Uniformity and the smallest dead volume.Upper cover 1 and chassis 2 are the designs of standard Luer mouth, so that with any sampling apparatus and admittedly
The connection of zero obstacle of phase extraction equipment.
Between upper cover 1 and chassis 2 is filtering/supporting layer 3 and extract layer 4.The molecule contained in bulk sample
Object can be removed by filter medium, prevent from being blocked in packing layer during extraction.Thickness, the material of filtering/supporting layer 3
Matter and particle size range can be adjusted according to the particulate matter degree of sample.Bulk sample, such as 5-10L sample are hoped per small
When treating capacity it is certainly The more the better, therefore the requirement for extraction stuffing is extraction efficiency height.The bioaccumulation efficiency of filler is got over
For high relative grain size with regard to smaller, resistance will be higher.When the particulate matter in sample is constantly assembled, it is easiest to block in extract layer, makes
It is interrupted at extraction.So the thickness of filtering/supporting layer 3 is bigger, partial size is smaller, it is better for the interception function of particulate matter.It can be with
According to actual sample, the combination of different size filtering/supporting layer 3 and extract layer 4 is formed.In addition to the effect of filtering, filtering/
Support layer 3 also acts as the effect of support, and the reticular structure that filter medium has has certain thickness, can be fixed by extract layer 4
In centre.The material of filtering/supporting layer 3 can be the similar filtering material such as micron-sized PP filter membrane, glass fiber filter.
Extraction stuffing in extract layer 4 can be the silica filler or polymer filler of various functional groups, such as C18, PS/
DVB, HLB etc..For the partial size of extraction stuffing in 10um-100um etc., particle size range is narrower, and the rate of recovery and stability are better.It is filling out
Expect that upper and lower surface places the filter disc that thickness is less than 0.5mm, 3-5mm lamella is pressed into together with filler.Due to solid phase of the invention
The upper cover 1 of extracting disk and chassis 2 are the designs of standard Luer mouth, it is of the invention can also by the chassis of multiple solid-phase extracting disks and
Upper cover is connected in series.There are also other three kinds of benefits for this design: 1) different types of extracting disk can be connected, realize many kinds of substance
While analyze；2) unknown sample when complicated component, the extracting disk of same type can be used in series, avoid the wind penetrated
Danger；3) thickness of filter layer and extraction stuffing can be adjusted according to actual sample, and the sample more for particulate matter can have needle
To the thickness of the increase filter layer of property, avoid interrupting in sampling process because resistance is excessive.Multiple series connection solid-phase extracting disks
Extraction stuffing and thickness can be with flexible choice, the partial size of the extraction stuffing is 10um-100um, the multiple series connection solid phase
The partial size of the extraction stuffing of extracting disk successively becomes smaller, to obtain the better rate of recovery and stability.
The present invention makes solid-phase extracting disk using ultrasonic bonding technology, and the shell of solid-phase extracting disk is by 2 liang of upper cover 1 and chassis
Part forms, and upper cover 1 and chassis 2 have separately designed symmetry liquid flow path.The inner surface on the i.e. described upper cover 1 and chassis 2 is circle
Disk, the liquid flow path is symmetrical along the radial direction of disc face, and the length of liquid flow path is adjacent in 10-25mm etc.
Angle between liquid flow path differs between 15-45 °, to guarantee the homogeneity of sample solution distribution, as shown in Figure 5.Bottom
Annular groove is additionally provided on disk 2.Annular groove is mainly two effects: first is that playing the role of bracket for filled layer, second is that annular
Slot itself is also the effect of drainage.Filter layer 3 between extract layer 4 and upper cover 1 has certain thickness and elasticity, and can be with
Realization is accurately cut out, and filter layer 3 can be filled between upper cover 1 and extract layer 4, guarantee that three combines closely, without gap.On
Lid 1 and chassis 2 are the designs of standard Luer mouth, so that connecting with any sampling apparatus and zero obstacle of solid-phase extraction device.Filtering/
Supporting layer 3 and extract layer 4 are filled layers, and filtering/supporting layer 3 and extract layer 4 are put into chassis 2, will by ultrasonic bonds
Upper cover 1 completes the production of solid-phase extracting disk together with 2 seamless welding of chassis.
The present invention can be realized with bulk sampling pipe, Solid Phase Extraction hand gear, Solid Phase Extraction full-automatic device it is light
Pine connection, meets the habit and mode of every kind of user.Data comparison is carried out by two experiments of AB again below.
It tests A:HLB (hydrophilic-hydrophobic balance) filler and tests tetracycline compound, comparison solid phase extraction column and solid phase extract
Take the rate of recovery and stability of disk.HLB pillar is classical SPE case for the enrichment of tetracycline compound in water.By with
The rate of recovery of pillar compares, the rate of recovery data that solid-phase extracting disk of the present invention obtains under the flow velocity of 50mL/min, can be perfect
Compared to the data under general SPE pillar gravity flow velocity, it was demonstrated that the advantage in its design and production, it was demonstrated that the design of extracting disk is closed
Reason, practicability reach requirement.The data comparison of solid-phase extracting disk and solid phase extraction column is as follows:
HPLC-UV detects following (HPLC- UV detection device):
| 10ppm standard items | 1 | 2 | Average value | The rate of recovery/% | The SPE pillar rate of recovery/% | |
| Terramycin | 297084 | 210956 | 212435 | 211695.5 | 71.26% | 73.16% |
| Tetracycline | 373894 | 275547 | 273792 | 274669.5 | 73.46% | 76.14% |
| Aureomycin | 148367 | 121451 | 100984 | 111217.5 | 74.96% | 73.56% |
It tests B:PS/DVB filler and tests phenol type substances, the Empore Solid Phase Extraction diaphragm and the present invention for comparing 3M extract
The rate of recovery and stability of disk, it was demonstrated that extracting disk of the invention is excellent as Empore Solid Phase Extraction diaphragm in performance.This
Invention solid-phase extracting disk and the data comparison of 3M Empore diaphragm are as follows:
GC/FID detects following (gas-chromatography/hydrogen flame detector):
The rate of recovery and 3M Empore diaphragm average recovery rate of solid-phase extracting disk of the present invention are close, have equivalent competition
Advantage, it is even better, illustrate that extracting disk effect is fine on the extraction ability of water sample with bulk mass.
Although the present invention is disclosed as above with preferred embodiment, however, it is not to limit the invention, any this field skill
Art personnel, without departing from the spirit and scope of the present invention, when can make a little modification and perfect therefore of the invention protection model
It encloses to work as and subject to the definition of the claims.
Claims (10)
1. a kind of solid-phase extracting disk for bulk sample, including the shell being made of upper cover (1) and chassis (2), feature
It is, the upper cover (1) and chassis (2) are bonded together by ultrasonic sealing, are set between the upper cover (1) and chassis (2)
Have extract layer (4), is provided with filtering/supporting layer (3), the upper cover between the extract layer (4) and upper cover (1), chassis (2)
(1) and the outer surface of chassis (2) is provided through standard Luer mouth, and the inner surface of the upper cover (1) and chassis (2) is provided with liquid
Body flow path.
2. being used for the solid-phase extracting disk of bulk sample as described in claim 1, which is characterized in that the upper cover (1) and bottom
The inner surface of disk (2) is disc face, and the liquid flow path is symmetrical along the radial direction of disc face, the length of the liquid flow path
Degree is 10-25mm, and 15 ° -45 ° of angle is formed between two neighboring liquid flow path.
3. as claimed in claim 2 be used for bulk sample solid-phase extracting disk, which is characterized in that the chassis (2) it is interior
Annular groove is also formed on surface, the annular groove is connected with radially-arranged liquid flow path.
4. being used for the solid-phase extracting disk of bulk sample as described in claim 1, which is characterized in that the upper cover (1) and bottom
The material of disk (2) is polypropylene.
5. being used for the solid-phase extracting disk of bulk sample as described in claim 1, which is characterized in that the filtering/supporting layer
(3) material is micron-sized PP filter membrane or glass fiber filter.
6. being used for the solid-phase extracting disk of bulk sample as described in claim 1, which is characterized in that in the extract layer (4)
Extraction stuffing be a variety of functional groups silica filler or polymer filler, the partial size of the extraction stuffing is 10um-100um,
The extraction stuffing upper and lower surface places the filter disc that thickness is less than 0.5mm, and the extraction stuffing suppresses shape together with upper and lower filter disc
At the lamellar structure of 3-5mm.
7. the Solid Phase Extraction processing method of a kind of bulk sample, using as claimed in any one of claims 1 to 6 for substantially
The solid-phase extracting disk of product sample, which is characterized in that the treating method comprises following steps:
A) select HLB or PSD as the extraction stuffing in extract layer (4)；
B) 5-10L sample is obtained, after activator and poising agent mixing is added, from upper cover (1) Rule mouth with 25mL/min-75mL/
The flow control mixed liquor of min enters solid-phase extracting disk；
C) after the completion of extracting, eluant, eluent cleaning is added.
8. the Solid Phase Extraction processing method of bulk sample as claimed in claim 7, which is characterized in that the step b) is added
As activator 15-30ml deionized water is added as poising agent, 15-30ml methanol is added in the step c) in 15-30ml methanol
Or 20-40ml methylene chloride is as eluant, eluent.
9. the Solid Phase Extraction processing method of bulk sample as claimed in claim 7, which is characterized in that further including will be multiple solid
The chassis (2) of phase extracting disk and upper cover (1) are connected in series.
10. the Solid Phase Extraction processing method of bulk sample as claimed in claim 9, which is characterized in that the extract layer (4)
In extraction stuffing be a variety of functional groups silica filler or polymer filler, the partial size of the extraction stuffing is 10um-
The partial size of 100um, the extraction stuffing of the multiple series connection solid-phase extracting disk successively become smaller.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710363877.0A CN108956258A (en) | 2017-05-22 | 2017-05-22 | Solid-phase extracting disk and its processing method for bulk sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710363877.0A CN108956258A (en) | 2017-05-22 | 2017-05-22 | Solid-phase extracting disk and its processing method for bulk sample |
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Cited By (1)
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| CN110579432A (en) * | 2019-09-24 | 2019-12-17 | 南京工业大学 | Dual-purpose sealing assembly and operation method |
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