CN105588872A - Quick on-line atmospheric photo ionization mass spectrum device for effective constituent in complex substrate - Google Patents
Quick on-line atmospheric photo ionization mass spectrum device for effective constituent in complex substrate Download PDFInfo
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- CN105588872A CN105588872A CN201610116956.7A CN201610116956A CN105588872A CN 105588872 A CN105588872 A CN 105588872A CN 201610116956 A CN201610116956 A CN 201610116956A CN 105588872 A CN105588872 A CN 105588872A
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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
- G01N27/64—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 wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
Abstract
The invention relates to a quick on-line atmospheric photo ionization mass spectrum device for an effective constituent in a complex substrate. The device comprises a pre-processing device, an atmospheric photo ionization source and a mass spectrometer, wherein the pre-processing device comprises an ultrasonic atomization mechanism, a volatile solvent introducing mechanism and a heating transfer mechanism. The device can be used for realizing the sensitive, quick and reliable qualitative and quantitative analysis after a to-be-detected sample containing complex substrate (such as, soil remained on explosion site, inferior milk power, food containing illegal additives, rootstocks of medicinal plants and the like) is directly put into the ultrasonic atomization mechanism and is subjected to ultrasonic atomization extraction, and then is delivered to and ionized at the front end of the atmospheric photo ionization source after being subjected to ultrasonic atomization and heating vaporization treatment and being converged with the volatile solvent. The device has wide application prospect at the aspects of discovery and identification of natural products, environment monitoring, criminal investigation, food safety, drug monitoring, etc.
Description
Technical field
The invention belongs to analysis technical field, be specially a kind of fast online atmospheric pressure photoionization mass spectrometric apparatus for complex matrices inside active ingredient.
Background technology
Compare with existing analysis means, especially spectral technique (such as infrared, ultraviolet, fluorescence etc.), mass spectral analysis is because its high sensitivity, high specific and high-throughout advantage more and more obtain people's attention in analytical chemistry field. Current discovery and qualification at natural products, environmental monitoring, criminal investigation, the aspects such as food security and drug monitoring, mass-spectrometric technique is widely used. But such as, due to common undressed sample substrate complexity (root, stem and leaf of explosion scene soil, milk powder inferior, the food that contains illegal additive and the medicinal plant left over etc.), before by mass spectral analysis, sample all needs conventionally through pretreatment process such as extraction, enrichment, chromatographic isolation, this process time and effort consuming, analysis cost is high.
Therefore, at earlier 2000s, someone has proposed can be used for the quick mass spectrometric analysis method of complex sample surface Direct Analysis, desorption electrospray MALDI-MS (DESI) and in real time Direct Analysis mass spectrum (DART). On this basis, a series of new mass spectrometric analysis methods are suggested and their unification are called to open type atmospheric pressure mass spectrum (AMS), comprise atmospheric pressure solid analysis probe mass spectrum (ASAP), low temperature plasma MALDI-MS (LTP) and ullrasonic spraying MALDI-MS (SSI) etc. In these methods, drop, thermal current or the plasma flow that compound can produce by spraying from the surface desorption of sample out, thereby detected by spectrometer analysis. But the ion or the plasma that mainly produce by electron spray ionisation, ullrasonic spraying ionization due to above-mentioned analytical method make compound ionization, low pole and nonpolar compound ionizing efficiency are lower; Secondly, as mentioned above, above-mentioned analytical method is to go out determinand by the surface desorption of the purging such as thermal current or plasma flow sample, thereby the material of matrix inside does not still desorb or desorption efficiency is very low, just be more difficult to realize for the quantitative analysis of matrix internalization compound so; On the other hand, in the process of desorb, (for example DESI) rushes at the surface of sample sometimes to need there is very strong air-flow, thereby cannot Direct Analysis for the sample (as soil, milk powder etc.) of Particle Phase, otherwise can bring serious pollution to instrument.
Summary of the invention
In order to solve the problem of above-mentioned existence, the invention provides a kind of fast online atmospheric pressure photoionization mass spectrometric apparatus for complex matrices inside active ingredient.
A kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient comprises pretreating device, atmospheric pressure photoionization source and mass spectrograph.
Described pretreating device comprises ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and adds heat transport mechanism.
Described ultrasonic atomizatio mechanism comprises ultrasonic atomizer 3, in the ultrasonic atomizatio chamber 6 of ultrasonic atomizer 3, is provided with extractant 4, and a side of ultrasonic atomizatio chamber 6 is being communicated with the first carrier gas pipe 1, the first carrier gas pipe 1 and is being provided with first flow meter 2.
Described solvent flashing retraction mechanism comprises solvent flashing storage tank 10, is provided with solvent flashing 9 in solvent flashing storage tank 10; The end that one side of solvent flashing storage tank 10 is being communicated with the second carrier gas pipe 7, the second carrier gas pipes 7 stretches in solvent flashing storage tank, and extend into below the liquid level of solvent flashing 9.
The described heat transport mechanism that adds comprises the supervisor 12 who keeps steady temperature, described supervisor's 12 entrance point is being communicated with the ultrasonic atomizatio chamber 6 of ultrasonic atomizer 3, supervisor 12 port of export correspondence the front end in mass spectrograph entrance 16 and atmospheric pressure photoionization source, and the outlet of solvent flashing storage tank 10 is being communicated with the middle part of being responsible for 12; Described supervisor's 12 temperature remains 200 ~ 500 DEG C.
Determinand 5 is located in the extractant 4 of ultrasonic atomizatio chamber 6;
Under positive ion mode, on mass spectrograph entrance 16, be applied with the voltage of-1 ~-6KV, the flow velocity of the dry gas 17 of mass spectrometric sample feeding pipe 18 outsides is at 3 ~ 10L/min, and temperature is at 100 ~ 400 DEG C.
The detailing further limiting is as follows:
Described atmospheric pressure photoionization source is VUV discharge lamp 15, and the outside of VUV discharge lamp is provided with the port of export of the 3rd carrier gas pipe 14, the three carrier gas pipes 14 facing to the bright dipping end of VUV discharge lamp, and the 3rd carrier gas pipe 14 is provided with the 3rd flowmeter 13.
Described mass spectrograph is flight time mass spectrum or level Four bar mass spectrum or ion trap mass spectrometry or Fourier transform ion cyclotron resonance mass spectroscopy or track trap mass spectrum or tandem mass spectrum.
On described supervisor 12, be arranged with heater strip 11, the internal diameter of supervisor 12 the port of export is at 1 ~ 4mm.
Described supervisor's 12 the port of export is parallel to mass spectrograph entrance 16, and the spacing of horizontal direction is 15 ~ 30mm between the two, and the spacing of vertical direction is 2 ~ 6mm, and the front end in described atmospheric pressure photoionization source is perpendicular to supervisor 12 the port of export.
Described supervisor's 12 the port of export is perpendicular to mass spectrograph entrance 16, and the spacing of horizontal direction is 5 ~ 30mm between the two, and the spacing of vertical direction is 2 ~ 10mm, and the front end in described atmospheric pressure photoionization source is vertical corresponding up and down with mass spectrograph entrance.
Described extractant 4 for first alcohol and water by volume 3:1 be mixed.
Described solvent flashing 9 for toluene and methyl phenyl ethers anisole by volume 1:1 be mixed.
Useful technique effect of the present invention embodies in the following areas:
1. apparatus of the present invention can be carried out Direct Analysis to the active ingredient of complex matrices inside, the such as jelly of soil, capsule, food, plant roots cauline leaf, animal tissue and thickness etc., the mass spectrogram of the orange peel internal component being obtained by the method from Fig. 3, the Main Flavonoids of orange peel inside and flavanone composition can be by fast detecting, as hesperetin (m/z303.08), orange peel element (m/z373.13), nobiletin (m/z403.14), Didymin (m/z595.20) and aurantiamarin (m/z611.19)。
Due to mass spectrograph entrance and supervisor's the port of export not point-blank, this device is in Direct Analysis Particle Phase, thickness phase sample, mass spectrograph can't be subject to serious pollution.
3. dry gas generally has the effect of desolventizing in mass spectrograph, in this device, can also make mass spectrometric vacuum system avoid the pollution of complex matrices.
4. this device is purging in the surperficial You Yi of VUV discharge lamp road carrier gas, this carrier gas has two effects, one can directly purge VUV discharge lamp surface and near pollutant, prevents that discharge lamp from being polluted, and ensures stability in use and the service life of discharge lamp; Its two surface at VUV discharge lamp forms one deck nitrogen protection layer, reduces the loss of photon in atmosphere, extends the propagation distance of photon in atmosphere, thereby improves photon utilization ratio and photo-ionisation efficiency.
5. this device all can effectively ionize for matrix inside polarity and nonpolar compound, without discrimination.
6. apparatus of the present invention can also be analyzed the compound direct quantitative of matrix inside, are used the linear relationship of pyrene in the soil that the method obtains by Fig. 4, and this linear coefficient correlation can reach 0.99602, visible, at 3-150ngmg-1Scope in the present invention can do quantitative analysis to the pyrene in soil.
Brief description of the drawings
Fig. 1 is when to be mass spectrograph entrance parallel with supervisor's the port of export, structural representation of the present invention.
Fig. 2 is when to be mass spectrograph entrance vertical with supervisor's the port of export, structural representation of the present invention.
Fig. 3 is under positive ion mode, using toluene as solvent flashing, and the mass spectrogram of the inner active ingredient of the orange peel of acquisition.
Fig. 4 is under positive ion mode, using toluene and methyl phenyl ethers anisole by volume 1:1 mix as solvent flashing, the linear relationship chart of pyrene in the soil of acquisition.
Sequence number in Fig. 1: the first carrier gas pipe 1, first flow meter 2, ultrasonic atomizer 3, extractant 4, determinand 5, ultrasonic atomizatio chamber 6, the second carrier gas pipe 7, the second flowmeter 8, solvent flashing 9, solvent flashing storage tank 10, heater strip 11, supervisor 12, the 3rd flowmeter 13, the 3rd carrier gas pipe 14, VUV discharge lamp 15, mass spectrograph entrance 16, dry gas 17, mass spectrograph sample feeding pipe 18.
Detailed description of the invention
Below in conjunction with accompanying drawing, by embodiment, the present invention is described further.
Embodiment 1
Referring to Fig. 1, comprise pretreating device, atmospheric pressure photoionization source and mass spectrograph for the fast online atmospheric pressure photoionization mass spectrometric apparatus of complex matrices inside active ingredient. Pretreating device comprises ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and adds heat transport mechanism. Atmospheric pressure photoionization source is VUV discharge lamp 15, and the outside of VUV discharge lamp 15 is provided with the port of export of the 3rd carrier gas pipe 14, the three carrier gas pipes 14 facing to the bright dipping end of VUV discharge lamp 15, and the 3rd flowmeter 13 is installed on the 3rd carrier gas pipe 14. Mass spectrograph is time of-flight mass spectrometer.
Ultrasonic atomizatio mechanism comprises ultrasonic atomizer 3, in the ultrasonic atomizatio chamber 6 of ultrasonic atomizer 3, extractant 4 is housed, extractant 4 for first alcohol and water by volume 3:1 be mixed, a side of ultrasonic atomizatio chamber 6 is being communicated with on the first carrier gas pipe 1, the first carrier gas pipe 1 first flow meter 2 is being installed.
Solvent flashing retraction mechanism comprises solvent flashing storage tank 10, and solvent flashing 9 is housed in solvent flashing storage tank 10, and solvent flashing 9 is toluene; The end that one side of solvent flashing storage tank 10 is being communicated with the second carrier gas pipe 7, the second carrier gas pipes 7 stretches in solvent flashing storage tank, and extend into below the liquid level of solvent flashing 9.
Add heat transport mechanism and comprise the supervisor 12 who keeps steady temperature, on supervisor 12, be arranged with heater strip 11, the internal diameter of supervisor 12 the port of export is 2mm. Supervisor 12 entrance point is being communicated with the ultrasonic atomizatio chamber 6 of ultrasonic atomizer 3, supervisor 12 port of export correspondence the front end in mass spectrograph entrance 16 and atmospheric pressure photoionization source, supervisor 12 the port of export is parallel to mass spectrograph entrance 16, the spacing of horizontal direction is 22mm between the two, the spacing of vertical direction is 3mm, and the bright dipping end of VUV discharge lamp 15 is perpendicular to supervisor 12 the port of export. The outlet of solvent flashing storage tank 10 is being communicated with the middle part of being responsible for 12; Supervisor 12 temperature remains 300 DEG C.
Determinand 5 is placed in the extractant 4 of ultrasonic atomizatio chamber 6.
Operation principle of the present invention is described as follows:
Determinand 5 is before mass spectral analysis, first will be responsible for 12 heating 10min, make the temperature stabilization of being responsible for 12 inwalls at 300 DEG C, then determinand 5 is placed in to the extractant 4 of ultrasonic atomizatio chamber 6, open ultrasonic atomizer 3 and regulate its input power, through ultrasonic atomizatio extraction 30 seconds, obtain vaporific extract; After having extracted, open atmospheric pressure photoionization source and mass spectrograph, open first flow meter 2, the second flowmeter 8 and the 3rd flowmeter 13 simultaneously, the nitrogen of inputting from the 3rd carrier gas pipe 14 blows to the surface of VUV discharge lamp 15, surface and near pollutant are purged totally, form one deck nitrogen protection layer on the surface of VUV discharge lamp simultaneously; The nitrogen of inputting from the first carrier gas pipe 1 is brought the vaporific extract in ultrasonic atomizatio chamber 6 into supervisor 12, the nitrogen of inputting from the second carrier gas pipe 7 is brought the solvent flashing in solvent flashing storage tank 10 9 into supervisor 12, converge with the extract of gasification, then the front end that arrives atmospheric pressure photoionization source by being responsible for 12 the port of export is ionized, the ion producing after ionization can, under the effect of electric field and pressure differential, enter the analyzed detection of mass analyzer in vacuum system by mass spectrograph entrance 16 and mass spectrograph sample feeding pipe 18. Under positive ion mode, the voltage of be applied with on mass spectrograph entrance 16-3.5KV, the flow velocity of the dry gas 17 of mass spectrometric sample feeding pipe 18 outsides is at 5L/min, and temperature is at 325 DEG C.
Embodiment 2
Referring to Fig. 2, mass spectrograph is level Four bar mass spectrograph. Extractant 4 for first alcohol and water by volume 3:1 be mixed, solvent flashing 9 for toluene and methyl phenyl ethers anisole by volume 1:1 be mixed;
Supervisor 12 the port of export is perpendicular to mass spectrograph entrance 16, and the spacing of horizontal direction is 15mm between the two, and the spacing of vertical direction is 3mm, and the bright dipping end of VUV discharge lamp 15 is vertical corresponding up and down with mass spectrograph entrance.
Under positive ion mode, the voltage of be applied with on mass spectrograph entrance 16-3.5KV, the flow velocity of the dry gas 17 of mass spectrometric sample feeding pipe 18 outsides is at 3.5L/min, and temperature is at 300 DEG C.
Other structure and operation principle are with embodiment 1.
Claims (8)
1. for a fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient, comprise pretreating device, atmospheric pressure photoionization source and mass spectrograph, it is characterized in that:
Described pretreating device comprises ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and adds heat transport mechanism;
Described ultrasonic atomizatio mechanism comprises ultrasonic atomizer (3), in the ultrasonic atomizatio chamber (6) of ultrasonic atomizer (3), be provided with extractant (4), one side of ultrasonic atomizatio chamber (6) is being communicated with the first carrier gas pipe (1), and the first carrier gas pipe (1) is provided with first flow meter (2);
Described solvent flashing retraction mechanism comprises solvent flashing storage tank (10), is provided with solvent flashing (9) in solvent flashing storage tank (10); One side of solvent flashing storage tank (10) is being communicated with the second carrier gas pipe (7), and the end of the second carrier gas pipe (7) stretches in solvent flashing storage tank, and extend into below the liquid level of solvent flashing (9);
The described heat transport mechanism that adds comprises the supervisor (12) who keeps steady temperature, described supervisor's (12) entrance point is being communicated with the ultrasonic atomizatio chamber (6) of ultrasonic atomizer (3), supervisor's (12) port of export correspondence the front end in mass spectrograph entrance (16) and atmospheric pressure photoionization source, and the outlet of solvent flashing storage tank (10) is being communicated with the middle part of supervisor (12); Described supervisor's (12) temperature remains 200 ~ 500 DEG C;
Determinand (5) is located in the extractant (4) of ultrasonic atomizatio chamber (6);
Under positive ion mode, on mass spectrograph entrance (16), be applied with the voltage of-1 ~-6KV, the flow velocity of the dry gas of mass spectrograph sample feeding pipe (18) outside is at 3 ~ 10L/min, and temperature is at 100 ~ 400 DEG C.
2. a kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient according to claim 1, it is characterized in that: described atmospheric pressure photoionization source is VUV discharge lamp (15), the outside of VUV discharge lamp is provided with the 3rd carrier gas pipe (14), the port of export of the 3rd carrier gas pipe (14) is facing to the bright dipping end of VUV discharge lamp, and the 3rd carrier gas pipe (14) is provided with the 3rd flowmeter (13).
3. a kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient according to claim 1, is characterized in that: described mass spectrograph is flight time mass spectrum or level Four bar mass spectrum or ion trap mass spectrometry or Fourier transform ion cyclotron resonance mass spectroscopy or track trap mass spectrum or tandem mass spectrum.
4. a kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient according to claim 1, it is characterized in that: on described supervisor (12), be arranged with heater strip (11), the internal diameter of supervisor's (12) the port of export is at 1 ~ 4mm.
5. a kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient according to claim 1, it is characterized in that: described supervisor's (12) the port of export is parallel to mass spectrograph entrance (16), the spacing of horizontal direction is 15 ~ 30mm between the two, the spacing of vertical direction is 2 ~ 6mm, and the front end in described atmospheric pressure photoionization source is perpendicular to supervisor's (12) the port of export.
6. a kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient according to claim 1, it is characterized in that: described supervisor's (12) the port of export is perpendicular to mass spectrograph entrance (16), the spacing of horizontal direction is 5 ~ 30mm between the two, the spacing of vertical direction is 2 ~ 10mm, and the front end in described atmospheric pressure photoionization source is vertical corresponding up and down with mass spectrograph entrance.
7. a kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient according to claim 1, is characterized in that: described extractant (4) for first alcohol and water by volume 3:1 be mixed.
8. a kind of fast online atmospheric pressure photoionization mass spectrometer for complex matrices active ingredient according to claim 1, is characterized in that: described solvent flashing (9) for toluene and methyl phenyl ethers anisole by volume 1:1 be mixed.
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