CN105588872B - A kind of quick online atmospheric pressure photoionization mass spectrometric apparatus for active ingredient in complex matrices - Google Patents
A kind of quick online atmospheric pressure photoionization mass spectrometric apparatus for active ingredient in complex matrices Download PDFInfo
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- 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
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Abstract
The present invention relates to a kind of quick online atmospheric pressure photoionization mass spectrometric apparatus for active ingredient inside complex matrices, the device includes pretreating device, atmospheric pressure photoionization source and mass spectrograph, and the pretreating device includes ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and heat transfer mechanism.The present invention can be by the sample to be tested containing complex matrices（The root, stem and leaf of soil, inferior milk power, the food containing illegal additive and medicinal plant that such as explosion scene is left）It direct plunges into ultrasonic atomizatio mechanism, after being extracted through ultrasonic atomizatio, after ultrasonic atomizatio and heating and gasifying processing, atmospheric pressure photoionization source front end is reached after with solvent flashing converging to be ionized, to realize sensitive, quick, reliable qualitative and quantitative analysis, in the discovery and identification of natural products, environmental monitoring, criminal investigation, food security and drug monitoring etc. have broad application prospects.
Description
Technical field
It is specially a kind of for the quick online big of complex matrices inside active ingredient the invention belongs to analysis technical field
Air pressure Photoionization Mass Spectrometry device.
Background technology
Compared to existing analysis means, especially spectral technique（Such as infrared, ultraviolet, fluorescence etc.）, mass spectral analysis by
The attention of people is increasingly obtained in analytical chemistry field in the advantage of its highly sensitive, high specific and high throughput.At present
In the discovery and identification of natural products, environmental monitoring, criminal investigation, food security and drug monitoring etc., mass-spectrometric technique
It has been obtained for being widely applied.However since common untreated sample substrate is complicated（Such as the soil that explosion scene is left
The root, stem and leaf etc. of earth, inferior milk power, the food containing illegal additive and medicinal plant）, before by mass spectral analysis, sample
It is usually required for by pretreatment process such as extraction, enrichment, chromatographic isolations, the process time and effort consuming, analysis cost is high.
Therefore, in earlier 2000s, it is thus proposed that can be used for the quick mass spectrum point that complex sample surface directly analyzes
Analysis method, desorption electrospray ionization mass spectrometry（DESI）With Direct Analysis in Real Time mass spectrum（DART）.On this basis, a series of new
Mass spectrometric analysis method is suggested and they is collectively referred to as open type atmospheric pressure mass spectrum（AMS）, including atmospheric pressure solid analysis
Probe mass spectrum（ASAP）, low temperature plasma ionization mass spectrometry（LTP）And ullrasonic spraying ionization mass spectrometry（SSI）Deng.In these sides
In method, compound can be come out by the spray drop, thermal current or the plasma flow that generate from the surface desorption of sample,
To be detected by spectrometer analysis.However since above-mentioned analysis method is mainly generated by electron spray ionisation, ullrasonic spraying ionization
Ion or plasma so that compound is ionized, low pole and nonpolar compound ionizing efficiency are relatively low；Secondly, institute as above
It states, above-mentioned analysis method is to go out determinand, thus base by the surface desorption of the purging sample such as thermal current or plasma flow
Substance inside matter does not desorb still or desorption efficiency is very low, then the quantitative analysis for content compound
Just more it is difficult to realize；On the other hand, during desorption, it is sometimes necessary to have very strong air-flow（Such as DESI）It rushes at
The surface of sample, thus for the sample of particle phase（Such as soil, milk powder）It can not directly analyze, otherwise can be brought to instrument sternly
The pollution of weight.
Invention content
It is above-mentioned in order to solve the problems, such as, the present invention provide it is a kind of for inside complex matrices active ingredient it is quick
Line atmospheric pressure photoionization mass spectrometric apparatus.
A kind of quick online atmospheric pressure photoionization mass spectrometer for active ingredient in complex matrices includes preceding place
Manage device, atmospheric pressure photoionization source and mass spectrograph.
The pretreating device includes ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and heat transfer mechanism.
The ultrasonic atomizatio mechanism includes ultrasonic atomizer 3, and it is molten to be equipped with extraction in the ultrasonic atomizatio room 6 of ultrasonic atomizer 3
The side of agent 4, ultrasonic atomizatio room 6 is connected to the first carrier gas pipe 1, and the first carrier gas pipe 1 is equipped with first flowmeter 2.
The solvent flashing retraction mechanism includes solvent flashing storage tank 10, and solvent flashing 9 is equipped in solvent flashing storage tank 10；
The side of solvent flashing storage tank 10 is connected to the second carrier gas pipe 7, and the end of the second carrier gas pipe 7 is stretched into solvent flashing storage tank, and
It extend into the liquid level of solvent flashing 9 or less.
The heat transfer mechanism includes keeping constant the supervisor 12 of temperature, and the input end of the supervisor 12 is connected to ultrasound
The ultrasonic atomizatio room 6 of atomizer 3, the outlet end for being responsible for 12 correspond to the front end of mass spectrometer inlet 16 and atmospheric pressure photoionization source,
The outlet of solvent flashing storage tank 10 middle part of supervisor 12；The temperature of the supervisor 12 remains 200 ~ 500 DEG C.
Determinand 5 is set in the extractant 4 of ultrasonic atomizatio room 6；
In the positive-ion mode, the voltage of -1 ~ -6 KV is applied on mass spectrometer inlet 16, outside mass spectrometric sample feeding pipe 18
The flow velocity of the drying gas 17 in portion is in 3 ~ 10 L/min, and temperature is at 100 ~ 400 DEG C.
The detailing further limited is as follows：
The atmospheric pressure photoionization source is vacuum ultraviolet discharge lamp 15, and the outside of vacuum ultraviolet discharge lamp is equipped with third carrier gas
Pipe 14, against the light extraction end of vacuum ultraviolet discharge lamp, third carrier gas pipe 14 is equipped with third stream for the outlet end of third carrier gas pipe 14
Gauge 13.
The mass spectrograph is flight time mass spectrum or level four bars mass spectrum or ion trap mass spectrometry or Fourier transformation ion involution
Resonate mass spectrum or Orbitrap mass or tandem mass spectrum.
It is arranged with heater strip 11 on the supervisor 12, is responsible for the internal diameter of 12 outlet end in 1 ~ 4mm.
The outlet end of the supervisor 12 is parallel to mass spectrometer inlet 16, and the spacing of horizontal direction is 15 ~ 30mm between the two,
The spacing of vertical direction is 2 ~ 6mm, and the front end in the atmospheric pressure photoionization source is perpendicular to the outlet end of supervisor 12.
The outlet end of the supervisor 12 is 5 ~ 30mm perpendicular to mass spectrometer inlet 16, the between the two spacing of horizontal direction,
The spacing of vertical direction is 2 ~ 10mm, and the front end in the atmospheric pressure photoionization source is vertical corresponding up and down with mass spectrometer inlet.
The extractant 4 is first alcohol and water by volume 3:1 is mixed.
The solvent flashing 9 is toluene and methyl phenyl ethers anisole by volume 1:1 is mixed.
The advantageous effects of the present invention embody in the following areas：
1. apparatus of the present invention can directly analyze the active ingredient inside complex matrices, such as soil, capsule, food
Product, plant roots cauline leaf, animal tissue and sticky jelly etc., by the matter of Fig. 3 orange peel internal components obtained with this method
Spectrogram is as it can be seen that Main Flavonoids and flavanone ingredient inside orange peel can be detected quickly, such as hesperetin（m/z
303.08）, orange peel element（m/z 373.13）, nobiletin（m/z 403.14）, Didymin（m/z595.20）And aurantiamarin（m/ z611.19）.
2. not point-blank due to the outlet end of mass spectrometer inlet and supervisor, which is directly analyzing particle
When phase, sticky phase sample, mass spectrograph can't be by serious pollution.
3. drying gas generally has the function of desolventizing in a mass spectrometer, in the apparatus, can also make mass spectrometric true
The pollution that empty set is united from complex matrices.
4. the device has carrier gas all the way purging on the surface of vacuum ultraviolet discharge lamp, effect that there are two carrier gas tools,
One can directly purge vacuum ultraviolet discharge lamp surface and neighbouring pollutant, and discharge lamp is prevented to be contaminated, and ensure discharge lamp
Stability in use and service life；Secondly forming one layer of nitrogen blanket on the surface of vacuum ultraviolet discharge lamp, photon is reduced
Loss in an atmosphere extends the propagation distance of photon in an atmosphere, to improve photon utilization ratio and photo-ionisation efficiency.
5. the device can effectively ionize content polarity with nonpolar compound, without discrimination.
6. apparatus of the present invention can also analyze the compound direct quantitative of content, obtained using this method by Fig. 4
Soil in pyrene linear relationship, the linear related coefficient is up to 0.99602, it is seen then that in 3-150 ng mg-1In the range of
The present invention can do quantitative analysis to the pyrene in soil.
Description of the drawings
When Fig. 1 is that mass spectrometer inlet is parallel with the outlet end of supervisor, schematic structural view of the invention.
When Fig. 2 is that mass spectrometer inlet is vertical with the outlet end of supervisor, schematic structural view of the invention.
Fig. 3 be in the positive-ion mode, using toluene as solvent flashing, the mass spectrum of the orange peel of acquisition inside active ingredient
Figure.
Fig. 4 is in the positive-ion mode, with toluene and methyl phenyl ethers anisole by volume 1:1 mixing is used as solvent flashing, acquisition
The linear relationship chart of pyrene in soil.
Serial number in Fig. 1：First carrier gas pipe 1, first flowmeter 2, ultrasonic atomizer 3, extractant 4, determinand 5, ultrasound
Spray chamber 6, the second carrier gas pipe 7, second flowmeter 8, solvent flashing 9, solvent flashing storage tank 10, heater strip 11, supervisor 12, third
Flowmeter 13, third carrier gas pipe 14, vacuum ultraviolet discharge lamp 15, mass spectrometer inlet 16, dry gas 17, mass spectrograph sample feeding pipe 18.
Specific implementation mode
Below in conjunction with the accompanying drawings, the present invention is described further by embodiment.
Embodiment 1
Referring to Fig. 1, before the quick online atmospheric pressure photoionization mass spectrometric apparatus for active ingredient inside complex matrices includes
Processing unit, atmospheric pressure photoionization source and mass spectrograph.Pretreating device include ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and
Heat transfer mechanism.Atmospheric pressure photoionization source is vacuum ultraviolet discharge lamp 15, and the outside of vacuum ultraviolet discharge lamp 15 is equipped with the
Three carrier gas pipes 14, the outlet end of third carrier gas pipe 14 are pacified on third carrier gas pipe 14 against the light extraction end of vacuum ultraviolet discharge lamp 15
Equipped with third flowmeter 13.Mass spectrograph is time of-flight mass spectrometer.
Ultrasonic atomizatio mechanism includes ultrasonic atomizer 3, and extractant 4 is housed in the ultrasonic atomizatio room 6 of ultrasonic atomizer 3,
Extractant 4 is first alcohol and water by volume 3:1 is mixed, and the side of ultrasonic atomizatio room 6 is connected to the first carrier gas pipe 1, the
First flowmeter 2 is installed on one carrier gas pipe 1.
Solvent flashing retraction mechanism includes solvent flashing storage tank 10, and solvent flashing 9, volatilization are housed in solvent flashing storage tank 10
Solvent 9 is toluene；The side of solvent flashing storage tank 10 is connected to the second carrier gas pipe 7, and it is molten that volatilization is stretched into the end of the second carrier gas pipe 7
In agent storage tank, and it extend into the liquid level of solvent flashing 9 or less.
Heat transfer mechanism includes keeping constant the supervisor 12 of temperature, is arranged with heater strip 11 on supervisor 12, is responsible for 12
The internal diameter of outlet end is 2mm.The input end of supervisor 12 is connected to the ultrasonic atomizatio room 6 of ultrasonic atomizer 3, is responsible for 12 outlet end
The front end for corresponding to mass spectrometer inlet 16 and atmospheric pressure photoionization source, the outlet end for being responsible for 12 are parallel to mass spectrometer inlet 16, and two
The spacing of horizontal direction is 22mm between person, and the spacing of vertical direction is 3mm, the light extraction end of vacuum ultraviolet discharge lamp 15 perpendicular to
The outlet end of supervisor 12.The outlet of solvent flashing storage tank 10 middle part of supervisor 12；The temperature of supervisor 12 remains 300
℃。
Determinand 5 is placed in the extractant 4 of ultrasonic atomizatio room 6.
The operation principle of the present invention is described as follows：
Supervisor 12 is heated 10min by determinand 5 first before through mass spectral analysis, so that the temperature of 12 inner wall of supervisor is stablized and is existed
300 DEG C, determinand 5 is then placed in the extractant 4 in ultrasonic atomizatio room 6, open ultrasonic atomizer 3 and adjusts its input work
Rate extracts 30 seconds through ultrasonic atomizatio, obtains misty extract liquor；After extraction is completed, atmospheric pressure photoionization source and mass spectrograph are opened,
First flowmeter 2, second flowmeter 8 and third flowmeter 13 are opened simultaneously, the nitrogen inputted from third carrier gas pipe 14 blows to very
The surface of empty EUV discharge lamp 15 purges on surface and neighbouring pollutant totally, while on the surface of vacuum ultraviolet discharge lamp
Form one layer of nitrogen blanket；The nitrogen inputted from the first carrier gas pipe 1 brings the misty extract liquor in ultrasonic atomizatio room 6 into supervisor
12, the nitrogen inputted from the second carrier gas pipe 7 brings the solvent flashing 9 in solvent flashing storage tank 10 into supervisor 12, the extraction with gasification
Liquid is taken to converge, the front end that atmospheric pressure photoionization source is then reached by the outlet end of supervisor 12 is ionized, what ionization generated later
Ion can be entered by mass spectrometer inlet 16 and mass spectrograph sample feeding pipe 18 under the action of electric field and pressure difference and be in vacuum system
The analyzed detection of mass analyzer.In the positive-ion mode, the voltage of -3.5 KV, mass spectrum are applied on mass spectrometer inlet 16
The flow velocity of drying gas 17 outside the sample feeding pipe 18 of instrument is in 5L/min, and temperature is at 325 DEG C.
Embodiment 2
Referring to Fig. 2, mass spectrograph is level four bars mass spectrograph.Extractant 4 is first alcohol and water by volume 3:1 is mixed,
Solvent flashing 9 is toluene and methyl phenyl ethers anisole by volume 1:1 is mixed；
The outlet end of supervisor 12 is 15mm, Vertical Square perpendicular to mass spectrometer inlet 16, the between the two spacing of horizontal direction
To spacing be 3mm, the light extraction end of vacuum ultraviolet discharge lamp 15 is vertical corresponding up and down with mass spectrometer inlet.
In the positive-ion mode, the voltage of -3.5 KV is applied on mass spectrometer inlet 16, outside mass spectrometric sample feeding pipe 18
Drying gas 17 flow velocity in 3.5L/min, temperature is at 300 DEG C.
Other structures and operation principle are the same as embodiment 1.
Claims (2)
1. a kind of quick online atmospheric pressure photoionization mass spectrometer for active ingredient in complex matrices, including pre-treatment
Device, atmospheric pressure photoionization source and mass spectrograph, it is characterised in that：
The pretreating device includes ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and heat transfer mechanism；
The ultrasonic atomizatio mechanism includes ultrasonic atomizer（3）, ultrasonic atomizer（3）Ultrasonic atomizatio room（6）It is interior to be equipped with extraction
Solvent（4）, ultrasonic atomizatio room（6）Side be connected to the first carrier gas pipe（1）, the first carrier gas pipe（1）It is equipped with first flowmeter
（2）；
The solvent flashing retraction mechanism includes solvent flashing storage tank（10）, solvent flashing storage tank（10）It is interior to be equipped with solvent flashing
（9）；Solvent flashing storage tank（10）Side be connected to the second carrier gas pipe（7）, the second carrier gas pipe（7）End stretch into solvent flashing
In storage tank, and it extend into solvent flashing（9）Liquid level below；The solvent flashing（9）For toluene and methyl phenyl ethers anisole by volume 1:1
It is mixed；
The heat transfer mechanism includes keeping constant the supervisor of temperature（12）, the supervisor（12）Input end be connected to ultrasound
Atomizer（3）Ultrasonic atomizatio room（6）, supervisor（12）Outlet end correspond to mass spectrometer inlet（16）With atmospheric pressure photoionization source
Front end, solvent flashing storage tank（10）Outlet supervisor（12）Middle part；The supervisor（12）On be arranged with heater strip
（11）, the supervisor（12）Temperature remain 200 ~ 500 DEG C；Supervisor（12）Outlet end internal diameter in 1 ~ 4mm；
The supervisor（12）Outlet end be parallel to mass spectrometer inlet（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 the atmospheric pressure photoionization source is perpendicular to supervisor（12）Outlet end；
The supervisor（12）Outlet end perpendicular to mass spectrometer inlet（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 the atmospheric pressure photoionization source is vertical corresponding up and down with mass spectrometer inlet；
The atmospheric pressure photoionization source is vacuum ultraviolet discharge lamp（15）, the outside of vacuum ultraviolet discharge lamp is equipped with third carrier gas pipe
（14）, third carrier gas pipe（14）Outlet end against the light extraction end of vacuum ultraviolet discharge lamp, third carrier gas pipe（14）It is equipped with the
Three flowmeters（13）；
Determinand（5）Set on ultrasonic atomizatio room（6）Extractant（4）In；The extractant（4）Volume is pressed for first alcohol and water
Than 3:1 is mixed；
In the positive-ion mode, mass spectrometer inlet（16）On be applied with the voltage of -1 ~ -6 KV, mass spectrograph sample feeding pipe（18）It is external
Drying gas flow velocity in 3 ~ 10 L/min, temperature is at 100 ~ 400 DEG C.
2. a kind of quick online atmospheric pressure photoionization mass spectrum for active ingredient in complex matrices according to claim 1
Analytical equipment, it is characterised in that：The mass spectrograph is flight time mass spectrum or level four bars mass spectrum or ion trap mass spectrometry or Fourier
Transform ion cyclotron resonance mass spectroscopy or Orbitrap mass or tandem mass spectrum.
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