CN111289602A - Feed detection device based on mass spectrometry technology and working method thereof - Google Patents
Feed detection device based on mass spectrometry technology and working method thereof Download PDFInfo
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- CN111289602A CN111289602A CN202010119424.5A CN202010119424A CN111289602A CN 111289602 A CN111289602 A CN 111289602A CN 202010119424 A CN202010119424 A CN 202010119424A CN 111289602 A CN111289602 A CN 111289602A
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- 238000001514 detection method Methods 0.000 title claims abstract description 71
- 238000004949 mass spectrometry Methods 0.000 title claims abstract description 29
- 238000005516 engineering process Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- IBXPYPUJPLLOIN-UHFFFAOYSA-N dimetridazole Chemical compound CC1=NC=C(N(=O)=O)N1C IBXPYPUJPLLOIN-UHFFFAOYSA-N 0.000 description 2
- 229960000946 dimetridazole Drugs 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- G01N27/626—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 using heat to ionise a gas
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (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 provides a feed detection device based on a mass spectrometry technology and a working method thereof, wherein the feed detection device based on the mass spectrometry technology comprises an ion source and a mass spectrometer; the bearing part is provided with fixing positions distributed along the center of the bearing part in a circumferential manner, and the fixing positions are suitable for fixing feed samples; the driving piece drives the bearing piece to rotate along the center of the bearing piece; the heating unit is used for heating the feed sample at the detection position; the feed sample at the detection position is not contacted with the plasma beam emitted by the ion source. The invention has the advantages of simple operation, high detection efficiency and the like.
Description
Technical Field
The invention relates to mass spectrometry, in particular to a feed detection device based on mass spectrometry technology and a working method thereof.
Background
The feed matrix is complex, a complex pretreatment process is required when the traditional liquid chromatography tandem mass spectrometry technology is used for detecting the antibiotics and other medicines in the feed, and the matrix interference is serious during detection. Common pretreatment methods are solid phase extraction, QuEChERS and the like, and after extraction and purification by using an organic solvent, complex steps such as nitrogen blowing concentration, solvent redissolution and the like are often needed, so that a large amount of organic reagents are consumed, the operation is complex, the cost is high, and the consumed time is long (more than 30 min). However, in general, the detection technology based on the open atmospheric pressure mass spectrometry ion source mostly adopts a one-step QuEChERS method for pretreatment and then solution sampling, so that the consumption of a large amount of organic solvents cannot be avoided, the cost is high, the time consumption is more than 10min, the background and matrix interference is serious, and the real rapid detection cannot be realized.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the feed detection device based on the mass spectrometry technology, which is simple to operate, high in detection efficiency and high in flux detection.
The purpose of the invention is realized by the following technical scheme:
a feed detection device based on mass spectrometry technology comprises an ion source and a mass spectrometer; the feed detection device based on the mass spectrometry technology further comprises:
a carrier having fixing locations circumferentially distributed along its center, the fixing locations adapted to fix a feed sample;
a driving member driving the bearing member to rotate along the center thereof;
the heating unit is used for heating the feed sample at the detection position; the feed sample at the detection position is not contacted with the plasma beam emitted by the ion source.
The invention also aims to provide a working method of the feed detection device based on the mass spectrometry technology, which is simple to operate, high in detection efficiency and low in detection cost, and the invention aims to be realized by the following technical scheme:
according to the working method of the feed detection device based on the mass spectrometry technology, the working method of the feed detection device based on the mass spectrometry technology comprises the following steps:
(A1) the dispersed feed samples were pressed into blocks with a density of 2g/cm3-3g/cm3；
(A2) The massive feed sample is fixed at the fixed position of the bearing part;
(A3) the block feed sample rotating along with the bearing piece reaches a detection position;
(A4) heating the block feed sample at the detection position to 573K-673K by a heating unit, and analyzing the components to be detected in the block feed sample;
(A5) and ionizing the component to be detected by a plasma beam emitted by the ion source, and analyzing the ionized component by the ion mass spectrometer, so as to obtain the content of the component to be detected in the feed.
Compared with the prior art, the invention has the beneficial effects that:
1. the influence of the uniformity of the block feed sample on the solvent analysis effect is small, the feed sample does not need to be homogenized and prepared, solid is directly injected after being pressed into blocks, the whole detection process can be finished within 1min, the cost and the time are saved to a great extent, and the operation complexity is reduced;
the density of the block sample has special requirements, and the volatilization of substances to be detected in the sample is influenced by too high density; too low a density, feed powder may enter the mass spectrometer; meanwhile, the heating temperature has special requirements, when the temperature is too low, high boiling point substances cannot be resolved out, and when the temperature is too high, a feed sample is carbonized, and too many impurities are introduced;
2. the trace organic solvent assists in resolving, and solvents with different proportions are selected according to different substances to be detected, so that the application is flexible;
3. the automatic single-step sample injection or continuous sample injection is realized by utilizing the rotary bearing piece and the arrangement of the detection position, the personal error is reduced, the cost and the time are saved, the method is simple, the operation is convenient, the detection efficiency is high, and the high-flux detection is realized;
the fixing positions are uniformly arranged on the circumference, so that the positioning difficulty of the sample is reduced, the angles of the bearing piece rotating every time are the same, and the control requirement is reduced;
4. only the bearing piece (the extension part) at the detection position is heated, other samples on the bearing piece cannot be influenced, the heating efficiency is improved, the heating time is short, and the detection efficiency is improved;
5. the device can be used with different model mass spectrometers, and the commonality is good.
Drawings
FIG. 1 is a schematic view of a feed testing device according to an embodiment of the present invention;
FIG. 2 is a flow chart of the operation of a feed detection device according to an embodiment of the present invention;
fig. 3 is a spectrum obtained according to an embodiment of the present invention.
Detailed Description
Fig. 1-3 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and use the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 schematically shows a schematic structural diagram of a feed detection device based on a mass spectrometry technology in embodiment 1 of the present invention, and as shown in fig. 1, the feed detection device based on the mass spectrometry technology includes:
an ion source 1 and a mass spectrometer 2, wherein the ion source 1 uses an open-type ion source under atmospheric pressure;
the bearing part 6 is provided with fixing positions 62 distributed along the center of the bearing part 6 in a circumferential manner, the fixing positions are suitable for fixing the feed sample pressed into a block shape, and if the fixing positions are grooves;
a driving member (not shown), such as a motor, which drives the carrier member to rotate along its center, thereby bringing different feed samples to the detection positions, respectively;
the heating unit 3 is used for heating the feed sample at the detection position; the feed sample at the detection position is not in contact with the plasma beam 5 emitted by the ion source.
In order to detect the component to be detected in the feed with high precision, further, the feed detection device further comprises:
and the liquid adding unit 4 is arranged above the detection position, and is not in contact with the plasma beam 5.
In order to avoid the heating unit from affecting the sample at the non-detection position, further, the carrier has a plurality of extensions 61 along the radial direction, and the fixing positions 62 are arranged on the extensions 61; the fixing site 62 is arranged at the end of the extension 61 remote from the centre of the carrier, so that the heating unit 3 only contacts and heats the extension 61 at the detection site, i.e. the sample is heated.
In order to reduce the difficulty of positioning and control, the fixing positions are further uniformly distributed along the circumferential direction which takes the center of the bearing part as the center of a circle, so that the angle of each rotation of the bearing part is the same.
In order to accurately apply the solvent to the sample on the fixed position, further, the central axis of the liquid adding unit and the central axis of the fixed position at the detection position are coincident.
Fig. 2 is a flow chart schematically showing a working method of a feed detection device based on a mass spectrometry technology in embodiment 1 of the present invention, and as shown in fig. 2, the working method comprises the following steps:
(A1) the dispersed feed samples are pressed into blocks, e.g. cylinders, with a density of 2g/cm3-3g/cm3；
(A2) The block feed sample is fixed at a fixed position of the bearing part, such as in a groove;
(A3) the block feed sample rotating along with the bearing piece reaches a detection position;
(A4) heating the block feed sample at the detection position to 573K-673K by a heating unit, and analyzing the components to be detected in the block feed sample; simultaneously, applying a solvent to the sample by using a liquid adding unit;
(A5) and ionizing the component to be detected by a plasma beam emitted by the ion source, and analyzing the ionized component by the ion mass spectrometer, so as to obtain the content of the component to be detected in the feed.
Example 2:
according to the feed detection device based on the mass spectrometry technology and the application example of the working method in the feed antibiotic detection, which are disclosed by the embodiment 1 of the invention.
In the application example, the ion source 1 adopts an open-type atmospheric pressure ion source, and the distance between the ion source 1 and the cone mouth of the mass spectrum analyzer 2 is 2 cm; the outer edge of the motor-driven carrier 6 has a plurality of extensions 61 uniformly distributed along the radial direction, and the end of the extensions 61 away from the center of the carrier has a groove serving as a fixing position 62 and suitable for accommodating a cylindrical block-shaped feed sample; the plasma beam 5 between the ion source and the cone mouth is parallel to the upper surface of the extension 61, and the distance is 4 mm; the liquid adding unit 4 adopts a liquid dropping device and is positioned above the plasma beam between the ion source and the cone mouth, and the central axis of the liquid dropping device is superposed with the central axis of the groove positioned at the detection position and is intersected with the plasma beam; the electric heating unit 3 is in contact with only the lower portion of the extension 61 at the detection position, and heats the feed sample in the groove by heat conduction.
The working method of the feed detection device based on the mass spectrometry technology comprises the following steps:
(A1) the dispersed feed samples are pressed into blocks, e.g. cylinders, with a density of 2g/cm3-3g/cm3E.g. 2g/cm3、2.3g/cm3、2.6g/cm3、3g/cm3Etc.;
(A2) the massive feed sample is fixed in the groove of the extension part, and the depth of the groove is greater than the height of the feed sample;
(A3) the block feed sample rotating along with the bearing piece reaches a detection position;
(A4) heating the block feed sample at the detection position to 573K-673K (573K, 602K, 640K and 673K) by a heating unit, and analyzing dimetridazole in the block feed sample; simultaneously, a solvent was applied to the sample using a dropper: dripping 50 mu L of methanol or acetonitrile at constant speed for 0.5s every 10 s;
(A5) the component to be detected is ionized by a plasma beam emitted by the ion source, the ion beam is transmitted to the mass spectrometer for analysis, a spectrogram is obtained, and the content of the dimetridazole in the feed is obtained by analyzing the spectrogram as shown in figure 3.
Claims (10)
1. A feed detection device based on mass spectrometry technology comprises an ion source and a mass spectrometer; the method is characterized in that: the feed detection device based on the mass spectrometry technology further comprises:
a carrier having fixing locations circumferentially distributed along its center, the fixing locations adapted to fix a feed sample;
a driving member driving the bearing member to rotate along the center thereof;
the heating unit is used for heating the feed sample at the detection position; the feed sample at the detection position is not contacted with the plasma beam emitted by the ion source.
2. The mass spectrometry-based feed detection device of claim 1, wherein: the fodder detection device still includes:
and the liquid adding unit is arranged above the detection position and is not in contact with the plasma beam.
3. The mass spectrometry-based feed detection device of claim 1, wherein: the fixing position is groove-shaped and is suitable for containing feed pressed into blocks.
4. The mass spectrometry-based feed detection device of claim 1, wherein: the carrier has a plurality of radially extending portions on which the securing locations are disposed.
5. The mass spectrometry-based feed detection device of claim 4, wherein: the fixing position is arranged at the end of the extension part far away from the center of the bearing part.
6. The mass spectrometry-based feed detection device of claim 1, wherein: the fixing positions are uniformly distributed along the circumferential direction which takes the center of the bearing part as the center of a circle.
7. The mass spectrometry-based feed detection device of claim 1, wherein: only the extension at the detection position is in contact with the heating unit at the lower side thereof.
8. The mass spectrometry-based feed detection device of claim 2, wherein: the central axis of the liquid adding unit is coincident with the central axis of the fixed position of the detection position.
9. The mass spectrometry-based feed detection device of claim 1, wherein: the plasma beam is parallel to the upper surface of the carrier.
10. The method of operating a mass spectrometry-based feed detection device as claimed in any one of claims 1 to 9, the method comprising the steps of:
(A1) the dispersed feed samples were pressed into blocks with a density of 2g/cm3-3g/cm3；
(A2) The massive feed sample is fixed at the fixed position of the bearing part;
(A3) the block feed sample rotating along with the bearing piece reaches a detection position;
(A4) heating the block feed sample at the detection position to 573K-673K by a heating unit, and analyzing the components to be detected in the block feed sample;
(A5) and ionizing the component to be detected by a plasma beam emitted by the ion source, and analyzing the ionized component by the ion mass spectrometer, so as to obtain the content of the component to be detected in the feed.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2019110195121 | 2019-10-24 | ||
| CN201911019512 | 2019-10-24 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111289602A true CN111289602A (en) | 2020-06-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010119424.5A Pending CN111289602A (en) | 2019-10-24 | 2020-02-26 | Feed detection device based on mass spectrometry technology and working method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN111289602A (en) |
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2020
- 2020-02-26 CN CN202010119424.5A patent/CN111289602A/en active Pending
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Country or region after: China Address after: West side of 1st floor, 1st floor, Building A, No. 288 Jingu Middle Road (East), Yinzhou District, Ningbo City, Zhejiang Province, 315000 Applicant after: CHINA INNOVATION INSTRUMENT Co.,Ltd. Applicant after: HUA YUE ENTERPRISE HOLDINGS Ltd. Address before: Room 304, D Building, Kexin Building, 655 Xueshi Road, Yinzhou District, Ningbo City, Zhejiang Province, 315000 Applicant before: CHINA INNOVATION INSTRUMENT Co.,Ltd. Country or region before: China Applicant before: HUA YUE ENTERPRISE HOLDINGS Ltd. |