CN202549785U - Electrospray ionization device - Google Patents

Electrospray ionization device Download PDF

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Publication number
CN202549785U
CN202549785U CN2012201287202U CN201220128720U CN202549785U CN 202549785 U CN202549785 U CN 202549785U CN 2012201287202 U CN2012201287202 U CN 2012201287202U CN 201220128720 U CN201220128720 U CN 201220128720U CN 202549785 U CN202549785 U CN 202549785U
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China
Prior art keywords
pipettor
filler
ionization
ionization device
electrospray ionization
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Expired - Fee Related
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CN2012201287202U
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Chinese (zh)
Inventor
冯钰锜
黄云清
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Wuhan University WHU
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Wuhan University WHU
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Abstract

The utility model relates to an electrospray ionization device which comprises a high-voltage power supply, a pipettor and a pipettor suction head connected with the pipettor and used for loading a filler, wherein the high-voltage power supply is connected with the pipettor suction head through a conductor. According to the electrospray ionization device adopting the structure, high voltage is directly applied to the pipettor suction head loaded with the filler, so that sample preparation and electrospray ionization can be completed on the electrospray ionization device, and interference of impurities in a complex sample to a target analyte and ionization inhibition are effectively reduced. The ionization device can be a handheld type and can also be assembled on an automatic manipulator, is convenient for use, and is beneficial to reduction of workload of people and increase of analysis flux.

Description

A kind of electro-spray ionization device
Technical field
The utility model relates to a kind of electro-spray ionization device.
Background technology
Mass spectrometer has high-resolution, high-sensitive advantage, and in food security, environmental protection is widely used in the analyzing and testing task in fields such as medicine and national security.When facing the analysis task of complex mixture, the common and chromatographic system coupling of mass spectrometer is to reduce signal interference and the signal suppressing of ambient interferences thing to analyte.Yet in the combined gas chromatography mass spectrometry analytic process, the preparation and the chromatographic isolation of sample have consumed great amount of time, thereby have limited the service speed of these analytical technologies.The part of this problem solves, and has benefited from fast-developing in the last few years normal pressure direct ionization technology, wherein, and desorption electrospray ionization method (Desorption Electrospray Ionization, DESI; " Science " magazine, the 306th volume, 471 pages (2004)) and real-time direct analysis (Direct Analysis in Real Time, DART; " Analytical Chemistry " magazine, the 77th volume, 2297 pages (2005)) be suggested at first.What both desorbs and ionization were used is that the former utilizes charged drop with a kind of energy carrier, and the latter utilizes low temperature plasma.Extract electro-spray ionization method (Extractive Electrospray Ionization, EESI in addition with desorption electrospray ionization method similar techniques; " Chemical Communications " magazine, 2042-2044 page or leaf (2006)) and receive liter extraction electro-spray ionization method (Nanoextractive Electrospray Ionization, a nanoEEI; " Analytical Chemistry " magazine, the 82nd volume, 7724-7731 page or leaf (2009)); Also have dielectric barrier discharge (Dielectric Barrier Discharge, DBDI with real-time direct analysis similar techniques; " Journal of the American Society for Mass Spectrometry " magazine, the 18th volume, 1859-1862 page or leaf (2007)), low temperature plasma probe (Low-Temperature Plasma Probe, LTP; " Analytical Chemistry " magazine, the 80th volume, 9098-9014 page or leaf (2008)) and the ionization of desorb corona beam (Desorption Corona Beam Ionization, DCBI; " Analyst " magazine, the 135th volume, 688-695 page or leaf (2010)).Desorb and ionization also appear in the newspapers with the ioning method of different energy carrier respectively and lead; For example; " Rapid Communication in Mass Spectrometry " magazine; The 19th volume, 3701-3704 page or leaf (2005) and " Rapid Communication in Mass Spectrometry " magazine, the 16th volume; It is the desorb means with laser that 681-685 page or leaf (2002) has been introduced a kind of respectively, is the normal pressure direct ionization technology of ionization instrument with charged drop or chemical ionization.Recently, multiplely do not need desorb, and directly sample is applied on the disposable carrier, realize that on disposable carrier Ionized technology also is developed, like paper spray technique (Paper Spray Ionization, PSI; " Angewandte Chemie" magazine, the 122nd volume, 889-892 page or leaf (2010)) and most advanced and sophisticated spray technique (the Electrospray Ionization Using Wooden Tips of toothpick; " Analytical Chemistry " magazine, the 83rd volume, 8201-8207 page or leaf (2011)).
Though the normal pressure direct ion technology of above introduction has obtained certain effect in the rapid analysis of urine, saliva, blood, skin and hair; But still face following problem: target analytes can be ionized with impurity simultaneously; On mass spectra peak, possibly there is overlapping peak, thus the accuracy of impact analysis; The inorganic ions that exists in the sample substrate or other organic chaff interferences have suppressed the desorption efficiency and the Ionization Efficiency of target analytes; Detection sensitivity still is apparent not enough.In order to improve the sensitivity and the selectivity of normal pressure direct ion fractional analysis technology; Can before carrying out ionization, carry out proper process to sample, i.e. sample preparation, yet; Introduce sample preparation; Certainly will need the cost more analysis time, need the extra used device of sample preparation, these all will cause the advantage of normal pressure direct ionization technology to be weakened.
The utility model content
The utility model technical problem to be solved provides a kind of electro-spray ionization device that can be complementary with sample preparation technology, on this electro-spray ionization device, can carry out sample preparation and ionization.
The utility model is the electro-spray ionization square law device that solve the technical problem, and comprises high voltage source, pipettor and the pipettor suction nozzle that is loaded with filler that is connected with pipettor, and said high voltage source is connected with the pipettor suction nozzle through conductor.
Said conductor is positioned at the top of said filler.
Perhaps, said conductor is positioned at the below of said filler.
The used high voltage source of the utility model electro-spray ionization device can be the high-pressure mini power supply, and is integrated on the said pipettor and is connected in aggregates with said pipettor.At this moment, as the improvement of this scheme, the voltage-regulation button can be set, voltage registration table and power switch button on pipettor.
The used high voltage source of the utility model electro-spray ionization device can also be external desk-top power supply or micro power.
The used pipettor of the utility model electro-spray ionization device is single channel pipettor or multichannel pipettor; Said pipettor can be hand-hold type, or is installed on upward use of automatic manipulator (comprising the manipulator that is connected with pipettor like said device).
Adopt the device of said structure, high voltage is applied directly on the pipettor suction nozzle that is loaded with filler, and sample preparation and electro-spray ionization are all accomplished on said device.Said ionization apparatus can use for hand-hold type also can be assembled to automation on hand, and is easy to use, and also helps to reduce people's workload, improves analysis throughput.
Description of drawings
Fig. 1 is the structural representation of the utility model.
Embodiment
The utility model provides the device of direct ionization under a kind of normal pressure.This device and sample preparation can well be mated, and have solved target analytes ionization in the complex sample analysis and have been suppressed the difficult problem that exists impurity to disturb with mass spectra peak.
Fig. 1 shows the structure that the utility model is realized the electro-spray ionization device.As shown in Figure 1, realize that the device of electro-spray ionization method comprises pipettor 1, high voltage source 2 is loaded with the pipettor suction nozzle 3 of filler, conductor 4.Wherein high voltage source 2 can be the high-pressure mini power supply, and is integrated on the said pipettor.At this moment, as the improvement of this scheme, voltage swing can be set on pipettor 1 regulate button 5, voltage registration table 6 and power switch button 7; High voltage source 2 can also be external desk-top power supply or micro power.The suction nozzle 3 that is loaded with filler is assemblied in the port of export of pipettor, and high voltage source links to each other through conductor 4 with suction nozzle.
The course of work of above-mentioned realization electro-spray ionization device is:
If the sample composition of being analyzed is simple, then the filler on the suction nozzle 3 preferably select for use with the target analytes effect a little less than material.For form is the sample of suspension-turbid liquid and neat liquid; Use said apparatus to draw small amount of sample; And the port of export of suction nozzle placed the mass spectrometer porch, and regulate button 5 through voltage swing and set required magnitude of voltage, turn on the power switch button 7; High-tension down auxiliary what applied, realize electro-spray ionization.For form is the sample (if the solid block sample, should earlier this solid sample be pulverized is pressed powder) of pressed powder, and the powder that takes a morsel is tiled on the sheet glass, forms skim, then powder is drawn in the suction nozzle 3 that is loaded with filler.After being loaded with the suction nozzle absorption pressed powder of filler, preferably sucking a spot of water or organic solution, and then carry out electro-spray ionization.
If the sample of analyzing is complicated, then the filler on the suction nozzle 3 is preferably selected the material stronger with the target analytes effect for use.Behind the pipettor 1 absorption sample through said apparatus, sample solution is discharged; Cleaning liquid suction is discharged cleaning fluid more then; Draw stripping liquid at last and carry out electro-spray ionization and Mass Spectrometer Method.Used stripping liquid volume not to be just in time having packing material, and exceeds the upper surface of packing material slightly, and connects suction nozzle 3 and contacts with the conductor of power supply 2 and be advisable.
The used pipettor 1 of said apparatus can be the hand-hold type pipettor, uses manual operations; Also can use operation automatically for being installed on automation pipettor on hand.At electro-spray ionization and when carrying out Mass Spectrometer Method; The angle of above-mentioned pipettor and mass spectrometer inlet is 0 °~90 ° variations; Do not influence the power of signal that mass spectrometer detects; This reappearance that target analytes will be detected is better, is more conducive to that also this device is installed on automated machine and uses on hand.
Application implementation example 1
10 μ L pipettor suction nozzles of the one filling porous silica gel material in tip buied are assembled on the electro-spray ionization device shown in Figure 1 (being that pipettor suction nozzle shown in Figure 1 is 10 μ L pipettor suction nozzles of the filling porous silica gel material in commercially available tip), draw 5 μ L pure water, 50% water-methanol (volume ratio), pure methyl alcohol, 50% water-acetonitrile (volume ratio) or pure acetonitrile.Voltage is set at+7.5 kV or-7.5 kV through regulation voltage size adjustment button, turns on the power switch button, high-tension down auxiliary what applied, the electron spray of umbrella appears in the tip of suction nozzle.
Embodiment 2
10 μ L pipettor suction nozzles of the one filling porous silica gel material in tip buied are assembled on the electro-spray ionization device shown in Figure 1, draw mixed solution (methanol-water, 1:1, the v/v of 5 μ L insorals, Pioglitazone and glibenclamide; Each component concentration is 200 ng/mL), voltage is set at+7.5 kV through regulation voltage size adjustment button, suction nozzle is placed mass spectrometer inlet top (vertical range 2 mm; Horizontal range 5 mm), pipettor and mass spectrometer inlet are 45, turn on the power switch button; High-tension down auxiliary what applied; The electron spray of umbrella appears in the tip of suction nozzle, simultaneously mass spectrometer detect three kinds of analytes mass signal (insoral, m/z 206; Pioglitazone, m/z 357; Glibenclamide, m/z 516).
Embodiment 3
10 μ L pipettor suction nozzles of one homemade tip filled glass fiber are assembled on the electro-spray ionization device shown in Figure 1, draw mixed solution (methanol-water, 1:1, the v/v of 5 μ L salicylic acids, jasmonic, heteroauxin, abscisic acid and gibberellin A 3; Each component concentration is 200 ng/mL), voltage is set at-7.5 kV through regulation voltage size adjustment button, other steps such as embodiment 2.Mass spectrometer detect five kinds of analytes mass signal (salicylic acid, m/z 137; Jasmonic, m/z 209; Heteroauxin, m/z 174; Abscisic acid, m/z 263; Gibberellin A 3, m/z 345).
Embodiment 4
10 μ L pipettor suction nozzles wiry are filled in one homemade tip be assembled on the electro-spray ionization device shown in Figure 1, draw the commercially available Coca-Cola of 5 μ L, voltage is set at+7.5 kV, other steps such as embodiment 2.Can be clearly seen that the signal (m/z, 195) of caffeine from the gained spectrogram.
More than combine accompanying drawing to disclose preferred embodiment of the utility model and embodiment; But the utility model is not limited to the above-described embodiment and examples; In spirit that does not break away from the utility model and scope, any those skilled in the art can also do some modification and perfect.

Claims (8)

1. electro-spray ionization device is characterized in that: comprise high voltage source, and pipettor and the pipettor suction nozzle that is loaded with filler that is connected with pipettor, said high voltage source is connected with the pipettor suction nozzle through conductor.
2. device as claimed in claim 1 is characterized in that: said conductor is positioned at the top of said filler.
3. device as claimed in claim 1 is characterized in that: said conductor is positioned at the below of said filler.
4. like claim 1 or 2 or 3 described devices, it is characterized in that: said high voltage source is the high-pressure mini power supply, and the high-pressure mini power supply is connected in aggregates with said pipettor.
5. like claim 1 or 2 or 3 described devices, it is characterized in that: said device also comprises the manipulator that is connected with pipettor.
6. like claim 1 or 2 or 3 described devices, it is characterized in that: said pipettor is provided with voltage-regulation button, voltage registration table and power switch button.
7. like claim 1 or 2 or 3 described devices, it is characterized in that: said pipettor is single channel pipettor or multichannel pipettor.
8. like claim 1 or 2 or 3 described devices, it is characterized in that: said pipettor is a hand-hold type.
CN2012201287202U 2012-03-30 2012-03-30 Electrospray ionization device Expired - Fee Related CN202549785U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106404885A (en) * 2015-07-28 2017-02-15 中国科学院化学研究所 Spraying system based on matrix-assisted laser desorption ionization mass spectrometry imaging, and biological sample analysis method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106404885A (en) * 2015-07-28 2017-02-15 中国科学院化学研究所 Spraying system based on matrix-assisted laser desorption ionization mass spectrometry imaging, and biological sample analysis method

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C17 Cessation of patent right
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Granted publication date: 20121121

Termination date: 20130330