CN107505383B - Quick extraction mass spectrum injector for pesticide residues - Google Patents
Quick extraction mass spectrum injector for pesticide residues Download PDFInfo
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- CN107505383B CN107505383B CN201710868652.0A CN201710868652A CN107505383B CN 107505383 B CN107505383 B CN 107505383B CN 201710868652 A CN201710868652 A CN 201710868652A CN 107505383 B CN107505383 B CN 107505383B
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- 239000000447 pesticide residue Substances 0.000 title claims abstract description 30
- 238000000605 extraction Methods 0.000 title claims abstract description 22
- 238000001819 mass spectrum Methods 0.000 title claims abstract description 15
- 239000000523 sample Substances 0.000 claims abstract description 64
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 24
- 238000009413 insulation Methods 0.000 claims abstract description 21
- 238000005070 sampling Methods 0.000 claims abstract description 21
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 39
- 238000005516 engineering process Methods 0.000 abstract description 12
- 238000007789 sealing Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 6
- 235000012055 fruits and vegetables Nutrition 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000012864 cross contamination Methods 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection 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
- 239000010959 steel Substances 0.000 description 1
Classifications
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- 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 a rapid extraction mass spectrum sampler for pesticide residues, which comprises a probe handle, a push rod, a solid phase extraction column, an injector and a sampling probe, wherein the probe handle comprises a handle lower part and a handle upper part, the solid phase extraction column is in sealing fit with the push rod, an extractant is arranged in an inner hole of the solid phase extraction column, the lower part of the inner hole of the solid phase extraction column is connected with a filtering device, the filtering device is connected with the upper part of the injector, the injector is connected with the upper part of the handle, an axial hole I is arranged at the lower part of the handle, a middle sleeve pipe is arranged in the axial hole I, an axial hole II is arranged in the middle sleeve pipe, an axial Kong Erna is provided with a heat insulation sleeve which is matched with the axial hole II, the outer cylindrical surface of the injector is matched with the middle hole and the axial hole III, and the injector is connected with the sampling probe. The invention has simple and compact structure, light weight, and low cost, and is convenient to operate, and the detection accuracy and efficiency of the thermal desorption-electrospray ion source technology are improved by combining the thermal desorption-electrospray ion source technology.
Description
Technical Field
The invention relates to the technical field of pesticide residue detection, in particular to a rapid extraction mass spectrum sampler for pesticide residues.
Background
There are various detection techniques for pesticide residues in the prior art, including the following two commonly used detection techniques:
firstly, the more popular pesticide residue detection technology in China needs to be realized by means of a liquid chromatograph or a gas chromatograph and other instruments, wherein a sample to be detected needs to be subjected to complex pretreatment, and the processing steps comprise: firstly, crushing an agricultural product sample, adding a certain solvent for extraction, injecting an extracting solution into an activated solid-phase extraction column, removing impurities, eluting pesticide residues by using a specific eluent, and allowing the eluent to enter a liquid chromatograph or a gas chromatograph through a filtering device and then enter a mass spectrometer for detection so as to ensure the sensitivity of detection and the accuracy of results. The defects and problems of the detection mode are that the pretreatment and analysis process of the detected sample requires a period of several hours, the process is complex, the time is long, the efficiency is low, and the working intensity of an operator is high.
Secondly, the detection technology used in foreign countries, especially European and American countries, is based on QuEChERS pretreatment, and the detection mode needs the following processing steps: crushing agricultural products, adding solvent for extraction, adding QuEChERS powder for adsorbing impurities, taking supernatant, filtering the supernatant by a filtering device, and then entering a liquid chromatograph or a gas chromatograph, and then entering a mass spectrometer.
In addition, the two methods in the prior art both require a complete set of detection equipment, including liquid phase, gas chromatograph and mass spectrometer. The equipment has large investment and high cost, occupies large space, has strong specialization, and operators need to be trained for a long time, which causes great inconvenience to quick law enforcement, especially quick pesticide residue detection of fruits and vegetables, and can not meet the special requirements of acquiring the detection result as soon as possible, then carrying out the next treatment according to the detection result or adopting the next measure.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a rapid extraction mass spectrum sample injector for pesticide residues; when the invention works, the detection sample after being subjected to homogeneous extraction can be placed into the inner hole of the solid phase extraction column, the detected sample is pressurized by the push rod and then is adsorbed with impurities and other accessories in the detection sample by the extractant, and pesticide residues remain to reach the position of the probe for further detection; the inner part and the outer part of the detected object can be directly sampled through the probe protuberance at the lower end of the probe body in a scraping mode and the like to directly carry out the next detection, and the extractant can not be filled at the moment. The internal pesticide residue and the external pesticide residue of the detected sample can be uniformly detected by both detection methods. The invention has simple and compact structure and light weight, combines the TD-ESI (thermal desorption-electrospray ion source) technology, improves the detection accuracy and efficiency of the TD-ESI technology, has low cost, reduces equipment investment and is convenient to operate.
The technical scheme for solving the technical problems is as follows:
the utility model provides a quick extraction mass spectrum sample injector of pesticide residue, includes probe handle, push rod, solid phase extraction post, filter equipment, syringe, intermediate sleeve, insulation cover, sampling probe, the probe handle includes handle lower part, takes the handle upper portion of intermediate hole, the hole surface and the push rod outer cylinder surface sealing fit of solid phase extraction post, is equipped with the extractant in the hole of solid phase extraction post, the hole lower part and the filter equipment of solid phase extraction post are connected, and filter equipment is connected with syringe upper portion, and the syringe is connected with handle upper portion, the handle lower part is equipped with axial hole one, be equipped with intermediate sleeve in the axial hole one, be equipped with axial hole two in the intermediate sleeve, axial Kong Erna is equipped with the insulation cover, the surface and the second cooperation of axial hole of insulation cover, the insulation cover is equipped with axial hole three, the outer cylinder of syringe respectively with the intermediate hole of handle upper portion, the axial hole three cooperation of handle lower part, the syringe is connected with sampling probe.
The injector comprises an upper sleeve with large diameter and a lower needle with small diameter and axial inner hole which are connected with each other, the lower part of the lower needle head is connected with the upper part of the sampling probe, the lower end of the sampling probe extends out of the heat insulation sleeve, and the lower end of the sampling probe is provided with a probe protrusion.
The solid phase extraction column comprises an upper cylinder body and a lower cylinder body, the diameter of the lower cylinder body is smaller than that of the upper cylinder body, and the lower end of the lower cylinder body is connected with the filtering device.
The outer wall of the lower part of the handle is provided with a heat insulation and anti-slip layer.
The middle sleeve adopts the metal tube, including inner tube, outer tube, be equipped with axial arch and recess cooperation between the outer wall of inner tube and the inner wall of outer tube, the inner tube can be followed the upper end of outer tube and taken out, and handle upper portion and inner tube connection are fixed as an organic wholely, and handle lower part and outer tube fixed connection are as an organic wholely.
The injector also comprises a boss at the upper part, the boss is connected with the upper end of the upper sleeve, and the boss is connected with the filtering device.
The extractant adopts FaPEx powder.
The probe protuberance is of a circular ring structure.
The probe body adopts a curve structure made of stainless steel wires, and the curve structure is contacted with the inner surface of the syringe needle and connected into a whole through friction force; the curve structure adopts a spiral spring structure, a sine function curve structure or a zigzag multi-line segment connection structure.
The heat insulation sleeve is made of ceramic materials with heat insulation effect.
The invention has the beneficial effects that:
1. the invention has simple and compact structure and light weight, combines the TD-ESI (thermal desorption-electrospray ion source) technology, improves the detection accuracy and efficiency of the TD-ESI technology, has low cost, reduces equipment investment, and is convenient to hold and operate.
2. When the invention works, the detection sample after being subjected to homogeneous extraction can be placed into the inner hole of the solid phase extraction column, the detected sample is pressurized by the push rod and then is adsorbed with impurities and other accessories in the detection sample by the extractant, and pesticide residues remain to reach the position of the probe for further detection; the inner part and the outer part of the detected object can be directly sampled through the probe protuberance at the lower end of the probe body in a scraping mode and the like to directly carry out the next detection, and the extractant can not be filled at the moment. The internal pesticide residue and the external pesticide residue of the detected sample can be uniformly detected by both detection methods, and the TD-ESI (thermal desorption-electrospray ion source) technology is combined, so that the detection accuracy of the TD-ESI technology is improved, the detection time is shortened, the equipment investment is reduced, the equipment volume is reduced, and the operation difficulty is reduced.
3. The structure of the rapid extraction mass spectrum sample injector for pesticide residues can be conveniently combined with TD-ESI, and the TD-ESI technology is selected to replace complex liquid phase gas chromatographic equipment, so that the problem that the TD-ESI technology in the prior art can only be suitable for a sample injection detection mode for detecting pesticide residues on the surface of a sample is solved, and the detection efficiency of the TD-ESI is improved. The whole sampling process can be completed within 2min to obtain the detection result, and the detection time is greatly shortened.
4. By using FaPEx powder extraction instead of the QuEChERs powder extraction technique, further improving the extraction efficiency and the accuracy of the detection result.
5. The invention can detect pesticide residues on the surfaces of fruits and vegetables and pesticide residues in the fruits and vegetables, simultaneously prevent a large amount of non-pesticide residue matrixes such as sugar, pigment and the like in the fruits and vegetables from entering the TD-ESI pollution ion source, and improve the accuracy and reliability of detection results.
6. The sampling probe adopts a detachable thin-wall cylinder and a matched probe body structure, the probe body adopts a curve structure made of stainless steel wires, and the probe body is connected with the inner surface of the syringe needle into a whole through a spiral spring structure, a sine function curve structure or a curve structure connected by zigzag multi-line sections in a contact manner by friction force.
7. Because form axial arch and recess cooperation between inner tube and the outer tube, the inner tube can be followed the upper end of outer tube and taken out, prevents the relative rotation between inner tube and the outer tube, and stability is good, guarantees that detection quality is reliable and stable.
8. Because push rod, solid phase extraction post, filter equipment, syringe, sampling probe are disposable product, need change new part and carry out the testing process of next time after once detecting, guaranteed that cross contamination can not take place in the continuous testing process, improved reliability and the efficiency of detecting. And the disposable product is convenient and quick to replace, the detection efficiency is improved, and the detection time is saved.
Drawings
FIG. 1 is a schematic diagram of the structure of the invention;
fig. 2 is a cross-sectional view of fig. 1.
Detailed Description
For a better understanding of the present invention, embodiments of the present invention are explained in detail below with reference to the drawings.
As shown in fig. 1 and 2, the quick extraction mass spectrum injector for pesticide residues comprises a probe handle, a push rod 1, a solid phase extraction column 2, a filtering device 3, a syringe 5, a middle sleeve 6, a heat insulation sleeve 8 and a sampling probe 9, wherein the probe handle comprises a handle lower part 7 and a handle upper part 4 with a middle hole, the inner hole surface of the solid phase extraction column 2 is in sealing fit with the outer cylinder surface of the push rod 1, an extractant 21 is arranged in the inner hole of the solid phase extraction column 2, the inner hole lower part of the solid phase extraction column 2 is connected with the filtering device 3, the filtering device 3 is connected with the upper part of the syringe 5, the syringe 5 is connected with the handle upper part 4, the handle lower part 7 is provided with an axial hole I, the middle sleeve 6 is internally provided with the middle sleeve 6, the middle sleeve 8 is axially provided with the heat insulation sleeve Kong Erna, the outer surface of the heat insulation sleeve 8 is matched with the axial hole II, the heat insulation sleeve 8 is provided with an axial hole III, and the outer cylinder surface of the syringe 5 is respectively matched with the middle hole of the handle upper part 4 and the axial hole III of the handle lower part 7.
The solid phase extraction column 2 comprises an upper cylinder 23 and a lower cylinder 22, the diameter of the lower cylinder being smaller than the diameter of the upper cylinder. The lower end of the lower cylinder body is connected with the filtering device 3.
The outer wall of the lower handle part 7 is provided with a heat insulation and anti-slip layer.
The middle sleeve 6 adopts a metal pipe and comprises an inner pipe 61 and an outer pipe 62, an axial protrusion and a groove are arranged between the outer wall of the inner pipe 61 and the inner wall of the outer pipe 62, the inner pipe 61 can be pulled out from the upper end of the outer pipe 62, the upper handle part 4 is connected and fixed with the inner pipe 61 into a whole, and the lower handle part 7 is fixedly connected with the outer pipe 62 into a whole. The inner tube 61 may be provided with a protrusion, the outer tube 62 may be provided with a groove, or the inner tube 61 may be provided with a groove, and the outer tube 62 may be provided with a protrusion, so that relative rotation between the inner tube and the outer tube is prevented. The middle sleeve is made of stainless steel, the outer tube and the lower part of the handle are fixed on the side face through screws, and grooves are formed in the middle sleeve, so that the inner tube 61 can be pulled up and down through matching of the protrusions and the grooves. The lower handle part 7 and the upper handle part 4 with the middle hole are made of plastic steel, and the upper handle part 4 and the inner tube are fixed up and down through screws, so that the upper handle part and the inner tube are pulled up and down together.
The injector 5 comprises an upper sleeve 52 with a large diameter and a lower needle 51 with a small diameter and an axial inner hole which are connected with each other, the lower part of the lower needle 51 is connected with the upper part of a sampling probe 9, the lower end of the sampling probe extends out of the heat insulation sleeve 8, and the lower end of the sampling probe is provided with a probe protrusion 91.
The syringe 5 further comprises an upper boss 53, the boss 53 being connected to the upper end of the upper sleeve 52, the boss 53 being connected to the filter means 3.
The extractant is FaPEx powder was used.
The probe protuberance is of a circular ring structure.
The probe body adopts a curve structure made of stainless steel wires, and the curve structure is contacted with the inner surface of the syringe needle and connected into a whole through friction force. The curve structure can adopt a spiral spring structure, a sine function curve structure or a zigzag multi-line segment connection structure.
Because push rod 1, solid phase extraction post 2, filter equipment 3, syringe 5, sampling probe 9 are disposable product, need to change new part and carry out the testing process of next time after once detecting, guaranteed that cross contamination can not take place in the continuous testing process, improved reliability and the efficiency of detecting. And the disposable product is convenient and quick to replace, the detection efficiency is improved, and the detection time is saved.
The heat insulation sleeve is made of ceramic materials with heat insulation effect, such as ceramic gaskets, so as to protect the lower part of the needle cylinder from being damaged by high temperature.
While the foregoing description of the embodiments of the present invention has been presented with reference to the drawings, it is not intended to limit the scope of the invention, but rather, it is apparent that various modifications or variations can be made by those skilled in the art without the need for inventive work on the basis of the technical solutions of the present invention.
Claims (7)
1. The utility model provides a quick extraction mass spectrum sample injector of pesticide residue, its characterized in that includes probe handle, push rod, solid phase extraction post, syringe, sampling probe, the probe handle includes handle lower part, the handle upper portion of taking the centre bore, the hole surface of solid phase extraction post and the sealed cooperation of push rod outer cylinder surface, be equipped with the extractant in the hole of solid phase extraction post, the hole lower part of solid phase extraction post is connected with filter equipment, and filter equipment is connected with syringe upper portion, and the syringe is connected with handle upper portion, the handle lower part is equipped with axial hole one, be equipped with the intermediate sleeve in the axial hole one, be equipped with axial hole two in the intermediate sleeve, axial Kong Erna is equipped with the insulating sleeve, the surface and the axial hole two of insulating sleeve cooperate, the insulating sleeve is equipped with axial hole three, the outer cylinder of syringe cooperates with the centre bore of handle upper portion, the axial hole three of handle lower part respectively, the syringe is connected with sampling probe;
the syringe comprises an upper sleeve with a large diameter and a lower needle with a small diameter and an axial inner hole which are connected with each other, the lower part of the lower needle is connected with the upper part of a sampling probe, the lower end of the sampling probe extends out of the heat insulation sleeve, and the lower end of the sampling probe is provided with a probe protrusion;
the solid phase extraction column comprises an upper cylinder and a lower cylinder which are connected, the diameter of the lower cylinder is smaller than that of the upper cylinder, and the lower end of the lower cylinder is connected with the filtering device;
the middle sleeve adopts the metal tube, including inner tube, outer tube, be equipped with axial arch and recess cooperation between the outer wall of inner tube and the inner wall of outer tube, the inner tube can be followed the upper end of outer tube and taken out, and handle upper portion and inner tube connection are fixed as an organic wholely, and handle lower part and outer tube fixed connection are as an organic wholely.
2. The rapid extraction mass spectrum injector for pesticide residues as claimed in claim 1, wherein the injector further comprises a boss at the upper part, the boss is connected with the upper end of the upper sleeve, and the boss is connected with the filtering device.
3. The rapid extraction mass spectrum injector for pesticide residues as set forth in claim 1, wherein the outer wall of the lower part of the handle is provided with a heat insulation and anti-slip layer.
4. The rapid extraction mass spectrum injector for pesticide residues according to claim 1, the method is characterized in that FaPEx powder is adopted as the extractant.
5. The rapid extraction mass spectrum injector for pesticide residues as set forth in claim 1, wherein the probe protrusion has a circular ring structure.
6. The rapid extraction mass spectrum sampler for pesticide residues as claimed in claim 1, wherein the sampling probe adopts a detachable thin-walled cylinder and a matched probe body structure, the probe body adopts a curve structure made of stainless steel wires, and the curve structure is contacted with the inner surface of a syringe needle and connected into a whole through friction force; the curve structure adopts a spiral spring structure, a sine function curve structure or a zigzag multi-line segment connection structure.
7. The rapid extraction mass spectrum injector for pesticide residues as set forth in claim 1, wherein the heat insulation sleeve is made of ceramic material with heat insulation effect.
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 |
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| Publication Number | Publication Date |
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| CN107505383A CN107505383A (en) | 2017-12-22 |
| CN107505383B true CN107505383B (en) | 2024-02-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710868652.0A Active CN107505383B (en) | 2017-09-22 | 2017-09-22 | Quick extraction mass spectrum injector for pesticide residues |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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|---|---|---|---|---|
| WO1992021393A1 (en) * | 1991-05-26 | 1992-12-10 | Arturo Moises Gotthelf | Safety device for medical syringe |
| CN102989432A (en) * | 2012-12-28 | 2013-03-27 | 南开大学 | Preparation of solid-phase microextraction (SPME) fiber and extraction device assembled by same |
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| CN207423881U (en) * | 2017-09-22 | 2018-05-29 | 山东国投鸿基检测技术股份有限公司 | A kind of pesticide residue Rapid Extraction mass spectrum injector |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6537827B1 (en) * | 1990-04-02 | 2003-03-25 | Janusz B. Pawliszyn | Method and device for solid phase microextraction and desorption |
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2017
- 2017-09-22 CN CN201710868652.0A patent/CN107505383B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO1992021393A1 (en) * | 1991-05-26 | 1992-12-10 | Arturo Moises Gotthelf | Safety device for medical syringe |
| CN102989432A (en) * | 2012-12-28 | 2013-03-27 | 南开大学 | Preparation of solid-phase microextraction (SPME) fiber and extraction device assembled by same |
| KR101471594B1 (en) * | 2013-06-24 | 2014-12-10 | 주식회사 씨피엘 | Injection purificating kit for injector |
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| CN107505383A (en) | 2017-12-22 |
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