CN107505383A - A kind of residues of pesticides Rapid Extraction mass spectrum injector - Google Patents
A kind of residues of pesticides Rapid Extraction mass spectrum injector Download PDFInfo
- Publication number
- CN107505383A CN107505383A CN201710868652.0A CN201710868652A CN107505383A CN 107505383 A CN107505383 A CN 107505383A CN 201710868652 A CN201710868652 A CN 201710868652A CN 107505383 A CN107505383 A CN 107505383A
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- residues
- syringe
- axial hole
- mass spectrum
- probe
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- 239000000575 pesticide Substances 0.000 title claims abstract description 25
- 238000000605 extraction Methods 0.000 title claims abstract description 20
- 238000001819 mass spectrum Methods 0.000 title claims abstract description 18
- 239000000523 sample Substances 0.000 claims abstract description 72
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 42
- 238000005516 engineering process Methods 0.000 abstract description 12
- 239000007921 spray Substances 0.000 abstract description 5
- 238000003795 desorption Methods 0.000 abstract 2
- 238000000034 method Methods 0.000 description 10
- 239000000284 extract Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 235000012055 fruits and vegetables Nutrition 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000002203 pretreatment Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000000447 pesticide residue Substances 0.000 description 3
- 238000007790 scraping Methods 0.000 description 3
- 239000003480 eluent Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses residues of pesticides Rapid Extraction mass spectrum injector, including probe handle, push rod, solid-phase extraction column, syringe, sample probe, probe handle includes lower portion thereof, handle upper portion, solid-phase extraction column coordinates with push rod seal, extractant is provided with the endoporus of solid-phase extraction column, the endoporus bottom of solid-phase extraction column is connected with filter, filter is connected with syringe top, syringe is connected with handle upper portion, lower portion thereof is provided with axial hole one, intermediate casing is provided with axial hole one, axial hole two is provided with intermediate casing, collet is provided with axial hole two, collet coordinates with axial hole two, collet is provided with axial hole three, the external cylindrical surface and interstitial hole of syringe, axial hole three coordinates, syringe is connected with sample probe.Simple and compact for structure, light weight of the invention, with reference to thermal desorption electric spray ion source technology, improves the Detection accuracy and efficiency of thermal desorption electric spray ion source technology, cost is low, equipment investment is few, easy to operation.
Description
Technical field
The present invention relates to the Detection Technologies of Pesticide Residues field, more particularly to a kind of residues of pesticides Rapid Extraction mass spectrum sample introduction
Device.
Background technology
The detection technique of prior art Pesticide Residues have it is a variety of, including following two kinds of conventional detection techniques：
First, the Detection Technologies of Pesticide Residues that China is more current, the detection technique is needed by liquid chromatograph or gas phase
The instruments such as chromatograph realize that the sample detected needed for it needs to include by complicated pre-treatment, processing step：Need first by
Agricultural samples crush, and add certain solvent extraction, the solid-phase extraction column after extract solution injection activation, remove impurity, afterwards
It is eluted out using specific eluent by agriculture is residual, eluent is entered into liquid chromatograph or gas-chromatography by filter
Instrument, detected subsequently into mass spectrograph, to ensure the accuracy of the sensitivity of detection and result.Existing for this detection mode
Defect and problem be, detected sample pre-treatments and analysis process need the time of several hours, and program is complicated, and process is numerous
Trivial, the time is long, efficiency is low, and operator's working strength is big.
Second, external particularly American-European current detection technique-detection technique based on QuEChERs pre-treatments, this inspection
Survey mode needs to carry out following processing step：Agricultural product are smashed, add solvent extraction, add the absorption of QuEChERs powder afterwards
Impurity, take supernatant to cross filter and enter liquid chromatograph or gas chromatograph, subsequently into mass spectrograph, with conventional method phase
Than, although the agricultural chemicals pre-treatment time reduced, program or it is complex, process is comparatively laborious, less efficient, it is impossible to
Enough requirements for meeting needs and obtaining testing result as early as possible.
The both the above method of other prior art, is required to a full set of detection device, including liquid phase, gas chromatograph and matter
Spectrometer.These equipment investments are big, cost is high, it is necessary to take larger space, and strongly professional, operating personnel are needed by long-term instruction
Practice, this puts to no little inconvenience to the residual detection of quick law enforcement, the particularly quick agriculture of fruits and vegetables, it is impossible to meets that needs obtain detection as early as possible
As a result and then according to testing result it is further processed or the situation of particular/special requirement using next step measure.
The content of the invention
For solving the above-mentioned problems of the prior art, it is an object of the present invention to provide a kind of residues of pesticides Rapid Extraction
Mass spectrum injector；Detection sample after homogeneous extracts can be put into the endoporus of solid-phase extraction column during present invention work, passed through
Sample is detected after push rod pressurization to adsorb impurity therein and other adjuncts by extractant, residues of pesticides are gone downwards to
Probe location carries out the detection of next step；Can also be directly by the probe projection of probe body lower end in detected article
Portion and the outside detection that directly progress next step is sampled by modes such as scrapings, can not now fill extractant.Pass through
Two kinds of detection methods can be detected equably to the inside residues of pesticides and outside residues of pesticides for being detected sample.This hair
Bright simple and compact for structure, light weight, TD-ESI (thermal desorption-electric spray ion source) technology is used in combination, improves TD-ESI skills
The Detection accuracy and efficiency of art, cost is low, reduces equipment investment, easy to operation.
The present invention solve technical problem technical scheme be：
A kind of residues of pesticides Rapid Extraction mass spectrum injector, including probe handle, push rod, solid-phase extraction column, filter,
Syringe, intermediate casing, collet, sample probe, the probe handle include lower portion thereof, the handle upper portion with interstitial hole,
The bore area of solid-phase extraction column coordinates with the sealing of push rod outer cylinder surface, and extractant, institute are provided with the endoporus of solid-phase extraction column
The endoporus bottom for stating solid-phase extraction column is connected with filter, and filter is connected with syringe top, on syringe and handle
Portion is connected, and the lower portion thereof is provided with axial hole one, and intermediate casing is provided with the axial hole one, is provided with axially in intermediate casing
Hole two, axial hole two is interior to be provided with collet, and outer surface and the axial hole two of collet coordinate, and the collet is provided with axial hole
Three, the interstitial hole with handle upper portion, the axial hole three of lower portion thereof coordinate the external cylindrical surface of the syringe respectively, the injection
Device is connected with sample probe.
The big upper sleeve of diameter of the syringe including interconnection, the small lower needle with axial bore of diameter
Head, the bottom of lower needle are connected with sample probe top, and collet is stretched out in sample probe lower end, and sample probe lower end, which is provided with, to be visited
Spicula rises.
Solid-phase extraction column includes top cylinder, lower cylinder, and the diameter of lower cylinder is less than the diameter of top cylinder, bottom
Cylinder lower end is connected with filter.
The outer wall of lower portion thereof is provided with heat-insulated and skid resistant course.
The intermediate casing uses metal tube, including inner tube, outer tube, is set between the outer wall of said inner tube and the inwall of outer tube
There is axial projection to coordinate with groove, inner tube can extract out from the upper end of outer tube, and handle upper portion is connected with inner tube and is integrated,
Lower portion thereof is connected to one with outer tube.
Syringe also includes the boss on top, the upper end connection of boss and upper sleeve, and boss is connected with filter.
The extractant uses FaPEx powder.
The probe projection is circular ring structure.
The probe body uses curvilinear structures made of stainless steel wire, and curvilinear structures contact logical with syringe needle inner surface
Frictional force is crossed to connect as one；The curvilinear structures are using helical spring structure, the tracks of line voltage structure or zigzag
Multi-thread section connection structure.
The collet is made up of the ceramic material with effect of heat insulation.
Beneficial effects of the present invention：
1. simple and compact for structure, light weight of the invention, is used in combination TD-ESI (thermal desorption-electric spray ion source) technology,
The Detection accuracy and efficiency of TD-ESI technologies are improved, cost is low, reduces equipment investment, and it is convenient, easy to operation to hold.
2. the detection sample after homogeneous extracts can be put into the endoporus of solid-phase extraction column, by pushing away during present invention work
Sample is detected after bar pressurization to adsorb impurity therein and other adjuncts by extractant, residues of pesticides go downwards to spy
Pin position carries out the detection of next step；Can also be directly by the probe projection of probe body lower end to the inside for the article being detected
The detection for directly carrying out next step is sampled by modes such as scrapings with outside, can not now fill extractant.Pass through two
Kind of detection method can be detected equably to the inside residues of pesticides and outside residues of pesticides for being detected sample, with reference to making
With TD-ESI (thermal desorption-electric spray ion source) technology, when improving the Detection accuracy of TD-ESI technologies, while shortening detection
Between, equipment investment is reduced, reduces equipment volume, reduces operation difficulty.
It is used in combination, passes through with TD-ESI 3. the residues of pesticides Rapid Extraction mass spectrum injector structure of the present invention can facilitate
From TD-ESI technologies to substitute the liquid phase gas chromatography apparatus of complexity, solve TD-ESI technologies in the prior art and be merely able to fit
The sample detection mode detected for scraping sample surfaces residues of pesticides, improve TD-ESI detection efficiency.Entirely take
Sample greatly shortens detection time to process can completion within 2min of testing result is obtained.
4. carrying out extraction by using FaPEx powder substitutes QuEChERs powder abstraction techniques, extraction is further increased
Efficiency and testing result accuracy.
5. the residual detection of agriculture that the present invention both can be to fruit and vegetable surfaces, can keep away the residual detection of agriculture inside fruits and vegetables simultaneously again
Exempt from the non-agricultural residue matter such as substantial amounts of carbohydrate, pigment in fruits and vegetables and enter TD-ESI contaminated ions source, improve the accurate of testing result
Property and reliability.
6. the sample probe of the present invention uses dismountable thin-walled cylinder and the probe body structure being engaged, probe body is adopted
The curvilinear structures made of stainless steel wire, pass through the multi-line section of helical spring structure, the tracks of line voltage structure or zigzag
The curvilinear structures of connection are contacted with syringe needle inner surface and connected as one by frictional force.
7. because the projection that axial direction is formed between inner tube and outer tube coordinates with groove, inner tube can take out from the upper end of outer tube
Go out, prevent the relative rotation between inner tube and outer tube, stability is good, ensures that detection steady quality is reliable.
8. because push rod, solid-phase extraction column, filter, syringe, sample probe are disposable products, one-time detection is complete
Carry out detection process next time again into the rear part for needing more to renew, ensure that will not occur to intersect in continuous detection process it is dirty
Dye, improve the reliability and efficiency of detection.And disposable products change fast and easy, improve detection efficiency, save
Detection time.
Brief description of the drawings
Fig. 1 is the structural representation of invention；
Fig. 2 is Fig. 1 sectional view.
Embodiment
For a better understanding of the present invention, embodiments of the present invention are explained in detail below in conjunction with the accompanying drawings.
Such as Fig. 1, shown in Fig. 2, a kind of residues of pesticides Rapid Extraction mass spectrum injector, including probe handle, push rod 1, solid phase
Extraction column 2, filter 3, syringe 5, intermediate casing 6, collet 8, sample probe 9, the probe handle are included under handle
Portion 7, the handle upper portion 4 with interstitial hole, bore area and the sealing of the outer cylinder surface of push rod 1 of solid-phase extraction column 2 coordinate, solid phase extraction
Take and extractant 21 is provided with the endoporus of post 2, the endoporus bottom of the solid-phase extraction column 2 is connected with filter 3, filter 3
It is connected with the top of syringe 5, syringe 5 is connected with handle upper portion 4, and the lower portion thereof 7 is provided with axial hole one, the axial hole
Intermediate casing 6 is provided with one, axial hole two is provided with intermediate casing 6, collet 8, the appearance of collet 8 are provided with axial hole two
Face coordinates with axial hole two, and the collet 8 is provided with axial hole three, the external cylindrical surface of the syringe 5 respectively with handle upper portion 4
Interstitial hole, the axial hole three of lower portion thereof 7 coordinates.
Solid-phase extraction column 2 includes top cylinder 22, lower cylinder 23, and the diameter of lower cylinder is less than the straight of top cylinder
Footpath.Lower cylinder lower end is connected with filter 3.
The outer wall of lower portion thereof 7 is provided with heat-insulated and skid resistant course.
The intermediate casing 6 uses metal tube, including inner tube 61, outer tube 62, outer wall and the outer tube 62 of said inner tube 61
The projection and groove that axial direction is provided between inwall coordinate, and inner tube 61 can extract out from the upper end of outer tube 62, handle upper portion 4 and inner tube
61, which are connected, is integrated, and lower portion thereof 7 is connected to one with outer tube 62.Projection can be set in inner tube 61, in outer tube
Groove is set on 62, groove can also be set in inner tube 61, sets projection on outer tube 62, prevents relative turn between inner tube and outer tube
It is dynamic.The intermediate casing is stainless steel, and outer tube is fixed with lower portion thereof by screw in side, and is provided with slideway, makes
Bosom sleeve pipe pull above and below slideway moves.The lower portion thereof 7, the handle upper portion 4 with interstitial hole are plastic-steel material, hand
Handle top 4 is fixed up and down by screw with inner tube, makes handle upper portion pull movement up and down together with inner tube.
The big upper sleeve 52 of diameter of the syringe 5 including interconnection, the small bottom with axial bore of diameter
Syringe needle 51, the bottom of lower needle 51 are connected with the top of sample probe 9, sample probe lower end stretching collet 8, under sample probe
End is provided with probe projection 91.
Syringe 5 also includes the boss 53 on top, and boss 53 is connected with the upper end of upper sleeve 52, and boss 53 fills with filtering
Put 3 connections.
The extractant uses FaPEx powder.
The probe projection is circular ring structure.
The probe body uses curvilinear structures made of stainless steel wire, and curvilinear structures contact logical with syringe needle inner surface
Frictional force is crossed to connect as one.Curvilinear structures can use helical spring structure, the tracks of line voltage structure or zigzag
Multi-thread section connection structure.
Because push rod 1, solid-phase extraction column 2, filter 3, syringe 5, sample probe 9 are disposable products, once examine
The part for needing more to renew after the completion of survey carries out detection process next time again, and ensure that in continuous detection process to hand over
Fork pollution, improve the reliability and efficiency of detection.And disposable products change fast and easy, improve detection efficiency, save
Detection time is saved.
The collet is made up of the ceramic material with effect of heat insulation, such as ceramic gasket, with protect syringe bottom not by
High temperature failure.
Although above-mentioned the embodiment of invention is described with reference to accompanying drawing, not to the scope of the present invention
Limitation, on the basis of technical scheme, those skilled in the art need not pay creative work and can make
Various modifications or deformation still within protection scope of the present invention.
Claims (10)
1. a kind of residues of pesticides Rapid Extraction mass spectrum injector, it is characterized in that, including probe handle, push rod, solid-phase extraction column, note
Emitter, sample probe, the probe handle include lower portion thereof, the handle upper portion with interstitial hole, the endoporus table of solid-phase extraction column
Face coordinates with the sealing of push rod outer cylinder surface, and extractant, the endoporus of the solid-phase extraction column are provided with the endoporus of solid-phase extraction column
Bottom is connected with filter, and filter is connected with syringe top, and syringe is connected with handle upper portion, the lower portion thereof
Provided with axial hole one, intermediate casing is provided with the axial hole one, axial hole two is provided with intermediate casing, is provided with axial hole two
Collet, outer surface and the axial hole two of collet coordinate, and the collet is provided with axial hole three, the outside cylinder of the syringe
The interstitial hole with handle upper portion, the axial hole three of lower portion thereof coordinate respectively in face, and the syringe is connected with sample probe.
2. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the syringe includes
The big upper sleeve of the diameter of interconnection, the small lower needle with axial bore of diameter, the bottom of lower needle and sampling
Probe top connects, and collet is stretched out in sample probe lower end, and sample probe lower end is provided with probe projection.
3. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 2, it is characterized in that, syringe also includes upper
The upper end connection of the boss in portion, boss and upper sleeve, boss are connected with filter.
4. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the solid-phase extraction column
Including top cylinder, the lower cylinder being connected, the diameter of lower cylinder is less than the diameter of top cylinder, lower cylinder lower end with
Filter connects.
5. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the intermediate casing is adopted
With metal tube, including inner tube, outer tube, the projection that axial direction is provided between the outer wall of said inner tube and the inwall of outer tube is matched somebody with somebody with groove
Close, inner tube can be extracted out from the upper end of outer tube, and handle upper portion is connected with inner tube and is integrated, and lower portion thereof is fixed with outer tube to be connected
It is connected in one.
6. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the lower portion thereof
Outer wall is provided with heat-insulated and skid resistant course.
7. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the extractant uses
FaPEx powder.
8. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the probe projection is
Circular ring structure.
9. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the probe body uses
Curvilinear structures made of stainless steel wire, curvilinear structures are contacted with syringe needle inner surface and connected as one by frictional force；Institute
State the multi-thread section connection structure that curvilinear structures use helical spring structure, the tracks of line voltage structure or zigzag.
10. a kind of residues of pesticides Rapid Extraction mass spectrum injector as claimed in claim 1, it is characterized in that, the collet is
Ceramic material with effect of heat insulation is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710868652.0A CN107505383B (en) | 2017-09-22 | 2017-09-22 | Quick extraction mass spectrum injector for pesticide residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710868652.0A CN107505383B (en) | 2017-09-22 | 2017-09-22 | Quick extraction mass spectrum injector for pesticide residues |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107505383A true CN107505383A (en) | 2017-12-22 |
| CN107505383B CN107505383B (en) | 2024-02-02 |
Family
ID=60697697
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710868652.0A Active CN107505383B (en) | 2017-09-22 | 2017-09-22 | Quick extraction mass spectrum injector for pesticide residues |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107505383B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982642A (en) * | 2018-05-24 | 2018-12-11 | 清华大学深圳研究生院 | A kind of method and device of jamming pattern signal when removing mass spectrograph sample introduction |
| CN110646544A (en) * | 2019-10-10 | 2020-01-03 | 山东省农业科学院农业质量标准与检测技术研究所 | Method for rapidly detecting pesticide residues in leaf vegetables |
| CN112924523A (en) * | 2021-01-28 | 2021-06-08 | 中国农业科学院农产品加工研究所 | Mass spectrum detection system and method with rapid extraction function for detecting pesticide residues |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982642A (en) * | 2018-05-24 | 2018-12-11 | 清华大学深圳研究生院 | A kind of method and device of jamming pattern signal when removing mass spectrograph sample introduction |
| CN108982642B (en) * | 2018-05-24 | 2020-09-25 | 清华大学深圳研究生院 | Method and device for removing interference background signal during sample injection of mass spectrometer |
| CN110646544A (en) * | 2019-10-10 | 2020-01-03 | 山东省农业科学院农业质量标准与检测技术研究所 | Method for rapidly detecting pesticide residues in leaf vegetables |
| CN112924523A (en) * | 2021-01-28 | 2021-06-08 | 中国农业科学院农产品加工研究所 | Mass spectrum detection system and method with rapid extraction function for detecting pesticide residues |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107505383B (en) | 2024-02-02 |
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