CN211125574U - Online reaction detection device based on double electric spray ion sources - Google Patents
Online reaction detection device based on double electric spray ion sources Download PDFInfo
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- CN211125574U CN211125574U CN202020258730.2U CN202020258730U CN211125574U CN 211125574 U CN211125574 U CN 211125574U CN 202020258730 U CN202020258730 U CN 202020258730U CN 211125574 U CN211125574 U CN 211125574U
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Abstract
The utility model provides an online reaction detection device based on two electric spray ion sources, includes ion source and mass spectrograph, the characteristic is: the ion source is provided with two sets of spraying components, one set of spraying components is used for spraying a sample solution to be detected, the other set of spraying components is used for spraying a derivatization reagent, the two sets of spraying components respectively comprise an injection pump, an injector and a spraying needle, the injector is connected with the spraying needle through a PEEK pipe, and the angle between the two spraying needles and the distance from the sampling cone opening of the mass spectrometer are adjustable. The utility model discloses extract the sample and the derivatization reagent that awaits measuring with two syringes respectively during the use, inject the spraying needle through the PEEK pipe through the syringe pump, sample and derivatization reagent atomize in the ion source, ionization and fast emergence reaction, then get into the mass spectrograph and carry out the analysis. The device has the greatest characteristic that the defects that a sample with poor stability and low ionization efficiency is difficult to directly detect and an indirect detection technology is time-consuming and labor-consuming are overcome through an in-source linear reaction technology, and the on-line and rapid detection of the substances is realized.
Description
Technical Field
The utility model relates to an used instrument of mass spectrometry technical field specifically is an online reaction detection device based on two electric spray ion sources.
Background
In recent years, the development of mass spectrum online detection technology is rapidly advanced, and the detection technology has the characteristics of simple and convenient operation, quick analysis, capability of realizing in-situ detection and good development and application prospects, but the application range of the detection technology is still limited to analytes with good stability and high ionization efficiency.
For analytes with strong volatility, high reactivity and low ionization efficiency, direct detection by a mass spectrometer is difficult due to poor stability or ionization efficiency, and the currently common detection method is to improve the stability and the ionization efficiency of the analytes by a derivatization technology, but the method is complicated to operate, consumes time and is labor-consuming.
Waters corporation developed an L ockSprayTMThe double electric spray ion source is used for improving the accurate mass number, and the schematic diagram of the device is shown in figures 1 and 2. The ion source is provided with two independent electrospray needles, a sample and correction liquid are atomized and ionized through the two electrospray needles respectively and enter the ion source, and the sample and the correction liquid alternately enter a sampling cone through an adjusting baffle. The disadvantage of this device is that the angle between the spray needles is not possibleAnd the plane where the two spray needles are positioned is parallel to the plane of the sample inlet, so that the sample injection rate is reduced, and the application range of the device is limited due to the existence of the baffle.
The currently common online derivatization apparatus is in-line derivatization, i.e. a sample and a derivatization reagent are mixed and reacted in a pipeline through a tee joint, and the schematic diagram of the apparatus is shown in fig. 3. The apparatus is generally comprised of a liquid chromatograph and a mass spectrometer, with a syringe pump injecting the derivatizing agent into the line. The disadvantage of this device is the long analysis time and the difficulty in accurately mixing the derivatizing reagent with the sample.
In order to realize the online rapid detection of analytes with high volatility, high reactivity and low ionization efficiency and widen the application range of mass spectrum online detection technology, an analysis device capable of overcoming the defects of the two detection technologies is urgently needed.
Disclosure of Invention
The utility model aims at providing an online reaction detection device based on two electric spray ion sources utilizes the device to carry out the online derivation in the source and detect to the analyte. The detection device combines the advantages of the mass spectrum on-line detection technology and the derivatization technology, is improved based on the existing ion source, widens the mass spectrum analysis range, and improves the analysis speed.
The purpose of the utility model is realized through the following technical scheme:
the utility model provides an online reaction detection device based on two electric spray ion sources, includes ion source and mass spectrograph, wherein: the ion source is provided with two sets of spraying components, one set of spraying components is used for spraying a sample solution to be detected, the other set of spraying components is used for spraying a derivatization reagent, the two sets of spraying components respectively comprise an injection pump, an injector and a spraying needle, the injector is connected with the spraying needle through a PEEK pipe, and the angle between the two spraying needles and the distance from the sampling cone opening of the mass spectrometer are adjustable.
The utility model discloses in, the angle between two spraying needles and apart from the distance of mass spectrograph sampling cone department adjust through two adjustment mechanism of fixing on the ion source shell respectively. The adjusting mechanism comprises an adjusting platform, a needle carrying platform, a ball bearing, an adjusting rod, a bevel gear pair and an annular buckle. The needle carrying table is connected with the table top of the adjusting table through a ball bearing and can rotate relative to the adjusting table, a driving bevel gear fixedly connected to the adjusting rod is meshed with a driven bevel gear fixed on the lower end face of the needle carrying table, two ends of the adjusting rod are respectively supported on two side walls of the lower portion of the adjusting table, a knob is arranged at one end of the adjusting rod, the driving bevel gear fixed on the adjusting rod is rotated by screwing the knob, the driven bevel gear and the needle carrying table are further driven to rotate, and finally the angle adjustment of the spray needle is realized; the two spray needles are fixed by an annular buckle arranged on the table top of the needle carrying table, and the distance between the two spray needles and the conical opening of the sampling cone can be adjusted.
According to different compounds, proper voltage polarity is selected, and the intensity and stability of the mass spectrum signal peak of the reaction product are realized by adjusting the angles of the two spraying needles, the distance between the two spraying needles and the sampling cone mouth and the applied voltage.
The PEEK tubing used to connect the syringe to the spray needle was as short as possible to reduce residue.
The injection pump is a single-channel pump, the adjustable flow rate range comprises 1-200 mu L/min, and the injector is a blunt injector with the capacity of 500 mu L.
Utilize the utility model discloses when examining, extract derivatization reagent and analysis sample with two syringes respectively, inject derivatization reagent and analysis sample into the ion source with the syringe pump, under the effect of spray voltage, derivatization reagent and analysis sample take place the ionization to the quick emergence reaction in the source, later get into the mass spectrum and carry out the analysis. The device has the greatest characteristics that the defects that a sample with poor stability and low ionization efficiency is difficult to directly detect and an indirect detection technology is time-consuming and labor-consuming are overcome through an in-source linear reaction technology, the online and rapid detection of the substances is realized, the range of detectable analytes is greatly widened, and the device has the advantages of simplicity and convenience in operation, stability and rapidness in analysis and capability of in-situ detection.
Drawings
FIG. 1 is a schematic diagram of a dual electrospray ion source in the prior art (when a calibration solution is ejected, a baffle blocks a sample ejection port).
Fig. 2 is a schematic diagram of a dual electrospray ion source in the prior art (when a sample solution is ejected, a baffle blocks an ejection port of a calibration solution).
FIG. 3 is a schematic diagram of a prior art in-line in-tube derivatization spray ion source.
Fig. 4 is a schematic structural diagram of the present invention.
Fig. 5 is a cross-sectional view of the spray needle adjustment device.
In fig. 4: the device comprises a sample solution, a derivatization reagent, a PEEK tube, 6-nitrogen, a spray needle, an 8-annular buckle, a 9-adjusting rod, a 10-adjusting platform, a 11-ball bearing, a 12-needle carrying platform, an ion source shell, a 14-double electric spray ion source, a 15-sampling cone opening and a 16-mass spectrometer, wherein the sample solution is prepared by a raw material preparation method of the sample solution, the derivatization reagent and the PEEK tube.
In fig. 5: 7-spray needle, 8-annular buckle, 9-adjusting rod, 9-1 driving bevel gear, 9-2 knob, 10-adjusting table, 11-ball bearing, 12-needle carrying table and 12-1 driven bevel gear.
Detailed Description
The utility model discloses the following further description of taking in conjunction with the figure:
as shown in fig. 4: an online reaction detection device based on a double-electric spray ion source comprises an ion source 14 and a mass spectrometer 16, wherein: the ion source 14 is provided with two sets of spraying components, one set of spraying components is used for spraying a sample solution 3 to be detected, the other set of spraying components is used for spraying a derivatization reagent 4, the two sets of spraying components comprise an injection pump 1, an injector 2 and a spraying needle 7, the injector 2 and the spraying needle 7 are connected through a peek pipe 5, and the angle between the two spraying needles 7 and the distance from the sampling cone mouth 15 of the mass spectrometer are adjustable.
The angle between two spray needles 7 and the distance from the sampling cone mouth 15 of the mass spectrometer are respectively adjusted through two adjusting mechanisms fixed on the ion source shell 13, and each adjusting mechanism comprises an adjusting platform 10, a needle carrying platform 12, a ball bearing 11, an adjusting rod 9, a bevel gear pair and an annular buckle 8. The needle carrying table 12 is connected with the top of the adjusting table 10 through a ball bearing 11 and can rotate relative to the adjusting table 10, a driving bevel gear 9-1 fixedly connected to the adjusting rod 9 is meshed with a driven bevel gear 12-1 fixed on the lower end face of the needle carrying table 12, two ends of the adjusting rod 9 are respectively supported on two side walls of the lower portion of the adjusting table 10, a knob 9-2 is arranged at one end of the adjusting rod 9, the driving bevel gear 12-1 fixed on the adjusting rod 9 is rotated by screwing the knob 9-2, the driven bevel gear 12-1 and the needle carrying table 12 are driven to rotate, and finally angle adjustment of the spray needle 7 is achieved. The two spray needles 7 are fixed by an annular buckle 8 arranged on the table surface of the needle carrying table 12, and the distance between the two spray needles and the sampling cone mouth 15 can be adjusted.
The two spray needles 7 are applied with voltages of the same polarity, and the magnitude and the positive and negative are respectively adjusted by an operating system. To reduce ion repulsion, the voltage of the spray needle ejecting the derivatizing agent is greater than the voltage of the spray needle ejecting the sample.
According to different compounds, the proper voltage polarity is selected, and the compatibility of the intensity and the stability of the mass spectrum signal peak of the reaction product is realized by adjusting the angles of the two spray needles 7, the distance between the two spray needles and the sampling cone mouth 15 and the magnitude of the applied voltage.
The PEEK tubing 5 used to connect the syringe 2 to the spray needle 7 is as short as possible to reduce residue.
The injection pump 1 is a single-channel pump, the adjustable flow rate range comprises 1-200 mu L/min, the injector 2 is a blunt injector, the capacity is 500 mu L, when the utility model is used, two injectors 2 are used for respectively extracting enough sample solution 3 and excessive derivatization reagent 4 and are connected to a PEEK pipe 5, and the two injectors 2 are respectively arranged on the two injection pumps 1.
Before detection, the ion source 14 and mass spectrometer 16 are activated, and then the syringe pump 1 is activated. The solution flows through a PEEK pipe 5 to enter a spray needle 7, is atomized and ionized under the action of nitrogen 6 and an electric field, then is mixed and reacted in an ion source 14, and the reaction product enters a mass spectrometer 16 through a sampling cone opening 15 for detection.
After the detection is completed, the syringe pump 1 is turned off, and then the ion source 14 and the mass spectrometer 16 are turned off. The remaining solution in the syringe 2 is injected into a waste bottle, cleaning the syringe 2 and the ion source 14.
Claims (6)
1. The utility model provides an online reaction detection device based on two electric spray ion sources, includes ion source and mass spectrograph, its characterized in that: the ion source is provided with two sets of spraying components, one set of spraying components is used for spraying a sample solution to be detected, the other set of spraying components is used for spraying a derivatization reagent, the two sets of spraying components respectively comprise an injection pump, an injector and a spraying needle, the injector is connected with the spraying needle through a PEEK pipe, and the angle between the two spraying needles and the distance from the sampling cone opening of the mass spectrometer are adjustable.
2. The on-line reaction detection device based on the dual electrospray ion source as recited in claim 1, characterized in that: voltage is applied to the two spray needles, and the size and the positive and negative of the two spray needles are respectively adjusted by an operating system.
3. The on-line reaction detection device based on the dual electrospray ion source as claimed in claim 2, characterized in that: the voltage of the spray needle ejecting the derivatizing agent is greater than the voltage of the spray needle ejecting the sample.
4. The on-line reaction detection device based on the dual electrospray ion source as recited in claim 1, characterized in that: the angle between the two spray needles and the distance from the sampling cone opening of the mass spectrometer are respectively adjusted by two adjusting mechanisms fixed on the ion source shell; the adjusting mechanism comprises an adjusting table, a needle carrying table, a ball bearing, an adjusting rod, a bevel gear pair and an annular buckle; the needle carrying table is connected with the table top of the adjusting table through a ball bearing and can rotate relative to the adjusting table, a driving bevel gear fixedly connected to the adjusting rod is meshed with a driven bevel gear fixed on the lower end face of the needle carrying table, two ends of the adjusting rod are respectively supported on two side walls of the lower portion of the adjusting table, a knob is arranged at one end of the adjusting rod, the driving bevel gear fixed on the adjusting rod is rotated by screwing the knob, the driven bevel gear and the needle carrying table are further driven to rotate, and finally the angle adjustment of the spray needle is realized; the two spray needles are fixed by an annular buckle arranged on the table top of the needle carrying table, and the distance between the two spray needles and the conical opening of the sampling cone can be adjusted.
5. The on-line reaction detection device based on the dual electrospray ion source as recited in claim 1, characterized in that: the peek tubing used to connect the syringe to the spray needle is as short as possible to reduce residue.
6. The on-line reaction detection device based on the dual-electric spray ion source as claimed in claim 1, wherein the injection pump is a single-channel pump, the adjustable flow rate range comprises 1-200 μ L/min, and the injector is a blunt injector with a capacity of 500 μ L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113205997A (en) * | 2021-05-06 | 2021-08-03 | 南京同歌网络科技有限公司 | Efficient ionization device for mass spectrometer |
| CN113267556A (en) * | 2021-07-19 | 2021-08-17 | 宁波大学 | Mobile drug detection system and method |
| CN113325063A (en) * | 2021-05-19 | 2021-08-31 | 宁波大学 | Device and method for verifying detection result of colloidal gold immunochromatographic test paper |
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2020
- 2020-03-05 CN CN202020258730.2U patent/CN211125574U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113205997A (en) * | 2021-05-06 | 2021-08-03 | 南京同歌网络科技有限公司 | Efficient ionization device for mass spectrometer |
| CN113205997B (en) * | 2021-05-06 | 2024-04-26 | 南京品生医疗科技有限公司 | Efficient ionization device for mass spectrometer |
| CN113325063A (en) * | 2021-05-19 | 2021-08-31 | 宁波大学 | Device and method for verifying detection result of colloidal gold immunochromatographic test paper |
| CN113325063B (en) * | 2021-05-19 | 2024-05-03 | 宁波大学 | Verifying device and method for colloidal gold immunochromatography test paper detection result |
| CN113267556A (en) * | 2021-07-19 | 2021-08-17 | 宁波大学 | Mobile drug detection system and method |
| CN113267556B (en) * | 2021-07-19 | 2021-11-02 | 宁波大学 | Mobile drug detection system and method |
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