CN205404478U - A quick online atmospheric pressure photo ionization mass spectrum device for active ingredient among complicated matrix - Google Patents
A quick online atmospheric pressure photo ionization mass spectrum device for active ingredient among complicated matrix Download PDFInfo
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- CN205404478U CN205404478U CN201620157680.2U CN201620157680U CN205404478U CN 205404478 U CN205404478 U CN 205404478U CN 201620157680 U CN201620157680 U CN 201620157680U CN 205404478 U CN205404478 U CN 205404478U
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Abstract
The utility model relates to an inside active ingredient's of complicated matrix quick online atmospheric pressure photo ionization mass spectrum device, the device include preceding processing apparatus, atmospheric pressure photo ionization source and mass spectrograph, preceding processing apparatus includes that ultrasonic atomization mechanism, volatile solvents introduce mechanism and heating transmission device. The utility model discloses can be with the need checking sample that contains complicated matrix (the soil of leaving over like the explosion scene, milk power inferior, contain the food of illegal additive and the rhizome leaf of medicinal plant etc. ) directly drop into in the ultrasonic atomization mechanism, after the ultrasonic atomization extraction, after ultrasonic atomization and heated gas ization processing, reach atmospheric pressure photo ionization source front end with volatile solvents after joiing by ionization, thereby realize sensitively, rapidness, reliable qualitative and quantitative analysis, discovery and appraisal at the natural products, the environmental monitoring, the criminal investigation, aspect such as food security and drug monitoring has wide application prospect.
Description
Technical field
This utility model belongs to analysis technical field, is specially a kind of quickly online atmospheric pressure photoionization mass spectrometric apparatus for complex matrices inside effective ingredient.
Background technology
With existing analysis means, especially spectral technique compares (such as infrared, ultraviolet, fluorescence etc.), and mass spectral analysis increasingly obtains the attention of people due to its high sensitivity, high specific and high-throughout advantage in analytical chemistry field.At present at the discovery of natural product and qualification, environmental monitoring, criminal investigation, the aspect such as food safety and drug monitoring, mass-spectrometric technique has been obtained for being widely applied.Yet with common undressed sample substrate complicated (root, stem and leaf etc. of soil that such as explosion scene is left over, inferior milk power, food containing illegal additive and medicinal plants), before by mass spectral analysis, sample is generally required for through pretreatment process such as extraction, enrichment, chromatographic isolation, this process time and effort consuming, analysis cost is high.
Therefore, at earlier 2000s, it is thus proposed that can be used for the quick mass spectrometric analysis method of complex sample surface direct analysis, desorption electrospray MALDI-MS (DESI) and Direct Analysis in Real Time mass spectrum (DART).On this basis, a series of new mass spectrometric analysis methods are suggested and they are collectively referred to as open type atmospheric pressure mass spectrum (AMS), including atmospheric pressure solid analysis probe mass spectrum (ASAP), low temperature plasma MALDI-MS (LTP) and ullrasonic spraying MALDI-MS (SSI) etc..In these methods, compound can pass through to spray the drop of generation, thermal current or plasma flow from the surface desorption of sample out, thus being detected by spectrometer analysis.Yet with above-mentioned analysis method mainly through electron spray ionisation, ullrasonic spraying ionization produce ion or plasma make compound ionize, low pole and nonpolar compound ionizing efficiency are relatively low；Secondly, as mentioned above, above-mentioned analysis method is to go out determinand by the surface desorption of the purging sample such as thermal current or plasma flow, thus the material of its content does not still desorb or desorption efficiency is very low, then the quantitative analysis for its content compound is just difficult to more；On the other hand, in the process of desorbing, it is sometimes necessary to have very strong air-flow (such as DESI) to rush at the surface of sample, thus for granule phase sample (such as soil, milk powder etc.) cannot direct analysis, otherwise can bring serious pollution to instrument.
Utility model content
In order to solve above-mentioned Problems existing, this utility model provides a kind of quickly online atmospheric pressure photoionization mass spectrometric apparatus for complex matrices inside effective ingredient.
A kind of include pretreating device, atmospheric pressure photoionization source and mass spectrograph for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices.
Described pretreating device includes ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and heat transfer mechanism.
Described ultrasonic atomizatio mechanism includes ultrasound atomizer 3, is provided with extractant 4 in the ultrasonic atomizatio room 6 of ultrasound atomizer 3, and the side of ultrasonic atomizatio room 6 connects the first carrier gas pipe 1, and the first carrier gas pipe 1 is provided with first-class gauge 2.
Described solvent flashing retraction mechanism includes solvent flashing storage tank 10, is provided with solvent flashing 9 in solvent flashing storage tank 10；The side of solvent flashing storage tank 10 connects 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.
Described heat transfer mechanism includes the supervisor 12 keeping steady temperature, the entrance point of described supervisor 12 connects the ultrasonic atomizatio room 6 of ultrasound atomizer 3, the port of export of supervisor 12 correspond to mass spectrometer inlet 16 and the front end in atmospheric pressure photoionization source, and the outlet of solvent flashing storage tank 10 middle part of supervisor 12；The temperature of described supervisor 12 remains 200 ~ 500 DEG C.
Determinand 5 is located in the extractant 4 of ultrasonic atomizatio room 6；
In the positive-ion mode, mass spectrometer inlet 16 being applied with the voltage of-1 ~-6KV, the flow velocity of the dry gas 17 outside mass spectrometric sample feeding pipe 18 is at 3 ~ 10L/min, and temperature is at 100 ~ 400 DEG C.
The detailing limited further is as follows:
Described atmospheric pressure photoionization source is VUV discharge lamp 15, and the outside of VUV discharge lamp is provided with the 3rd carrier gas pipe 14, and the port of export of the 3rd carrier gas pipe 14 goes out light end facing to VUV discharge lamp, and the 3rd carrier gas pipe 14 is provided with the 3rd effusion meter 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 Orbitrap mass or tandem mass spectrum.
Being arranged with heater strip 11 on described supervisor 12, the internal diameter of the port of export of supervisor 12 is at 1 ~ 4mm.
The port of export of described supervisor 12 is parallel to mass spectrometer inlet 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 the port of export of supervisor 12.
The port of export of described supervisor 12 is perpendicular to mass spectrometer inlet 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 spectrometer inlet.
Described extractant 4 is mixed for first alcohol and water 3:1 by volume.
Described solvent flashing 9 is mixed for toluene and methyl phenyl ethers anisole 1:1 by volume.
Advantageous Effects of the present utility model is embodied in following aspect:
1. the effective ingredient within complex matrices can be carried out direct analysis by this utility model device, the jelly etc. of such as soil, capsule, food, plant roots stem and leaf, animal tissue and thickness, the mass spectrum of the orange peel internal component obtained from Fig. 3 the method, Main Flavonoids and flavanone composition within orange peel can quickly be detected, as hesperetin (m/z303.08), Pericarpium Citri tangerinae element (m/z373.13), nobiletin (m/z403.14), Didymin (m/z595.20) and Hesperidin (m/z611.19).
2. due to the port of export of mass spectrometer inlet and supervisor not point-blank, this device is when direct analysis granule phase, thickness phase sample, and mass spectrograph can't be subject to serious pollution.
3. dry gas generally has the effect of desolventizing in a mass spectrometer, in the apparatus, it is also possible to make mass spectrometric vacuum system from the pollution of complex matrices.
4. this device has a road-load gas purging on the surface of VUV discharge lamp, this carrier gas has two effects, one can directly purge VUV discharge lamp surface and neighbouring pollutant, it is prevented that discharge lamp is contaminated, it is ensured that the stability in use of discharge lamp and service life；Its two the surface of VUV discharge lamp formed one layer of nitrogen blanket, reduce photon loss in an atmosphere, extend photon propagation distance in an atmosphere, thus improving photon utilization ratio and photo-ionisation efficiency.
5. this device all can effectively ionize for its content polarity and nonpolar compound, without discrimination.
6. the compound direct quantitative of its content can also be analyzed by this utility model device, Fig. 4 linear relationship of pyrene in the soil using the method to obtain, and this linear correlation coefficient is up to 0.99602, it is seen then that at 3-150ngmg-1Scope in this utility model the pyrene in soil can be done quantitative analysis.
Accompanying drawing explanation
Fig. 1 be mass spectrometer inlet parallel with the port of export of supervisor time, this utility model structural representation.
Fig. 2 be mass spectrometer inlet vertical with the port of export of supervisor time, this utility model structural representation.
Fig. 3 is in the positive-ion mode, using toluene as solvent flashing, it is thus achieved that the mass spectrum of the internal effective ingredient of orange peel.
Fig. 4 is in the positive-ion mode, mixes as solvent flashing using toluene and methyl phenyl ethers anisole 1:1 by volume, it is thus achieved that soil in the linear relationship chart of pyrene.
Sequence number in Fig. 1: the first carrier gas pipe 1, first-class gauge 2, ultrasound atomizer 3, extractant 4, determinand 5, ultrasonic atomizatio room the 6, second carrier gas pipe 7, second gauge 8, solvent flashing 9, solvent flashing storage tank 10, heater strip 11, supervisor's the 12, the 3rd effusion meter the 13, the 3rd carrier gas pipe 14, VUV discharge lamp 15, mass spectrometer inlet 16, dry gas 17, mass spectrograph sample feeding pipe 18.
Detailed description of the invention
Below in conjunction with accompanying drawing, by embodiment, this utility model is described further.
Embodiment 1
Referring to Fig. 1, the quickly online atmospheric pressure photoionization mass spectrometric apparatus for complex matrices inside effective ingredient includes pretreating device, atmospheric pressure photoionization source and mass spectrograph.Pretreating device includes ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and heat transfer mechanism.Atmospheric pressure photoionization source is VUV discharge lamp 15, and the outside of VUV discharge lamp 15 is provided with the 3rd carrier gas pipe 14, and the port of export of the 3rd carrier gas pipe 14 goes out light end facing to VUV discharge lamp 15, and the 3rd carrier gas pipe 14 is provided with the 3rd effusion meter 13.Mass spectrograph is time of-flight mass spectrometer.
Ultrasonic atomizatio mechanism includes ultrasound atomizer 3, the ultrasonic atomizatio room 6 of ultrasound atomizer 3 is built with extractant 4, extractant 4 is mixed for first alcohol and water 3:1 by volume, and the side of ultrasonic atomizatio room 6 connects the first carrier gas pipe 1, and the first carrier gas pipe 1 is provided with first-class gauge 2.
Solvent flashing retraction mechanism includes solvent flashing storage tank 10, and solvent flashing storage tank 10 is built with solvent flashing 9, and solvent flashing 9 is toluene；The side of solvent flashing storage tank 10 connects 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.
Heat transfer mechanism includes the supervisor 12 keeping steady temperature, and supervisor 12 is arranged with heater strip 11, and the internal diameter of the port of export of supervisor 12 is 2mm.The entrance point of supervisor 12 connects the ultrasonic atomizatio room 6 of ultrasound atomizer 3, the port of export of supervisor 12 correspond to mass spectrometer inlet 16 and the front end in atmospheric pressure photoionization source, the port of export of supervisor 12 is parallel to mass spectrometer inlet 16, the spacing of horizontal direction is 22mm between the two, the spacing of vertical direction is 3mm, and the light end that goes out of VUV discharge lamp 15 is perpendicular to the port of export of supervisor 12.The outlet of solvent flashing storage tank 10 middle part of supervisor 12；The temperature of supervisor 12 remains 300 DEG C.
Determinand 5 is placed in the extractant 4 of ultrasonic atomizatio room 6.
Operation principle of the present utility model illustrates as follows:
Determinand 5 is before mass spectral analysis, first supervisor 12 is heated 10min, make the temperature stabilization of supervisor 12 inwall at 300 DEG C, then determinand 5 is placed in the extractant 4 in ultrasonic atomizatio room 6, open ultrasound atomizer 3 and regulate its input power, extract 30 seconds through ultrasonic atomizatio, obtain vaporific extract；After extraction completes; open atmospheric pressure photoionization source and mass spectrograph; open first-class gauge 2, second gauge 8 and the 3rd effusion meter 13 simultaneously; the surface of VUV discharge lamp 15 is blowed to from the nitrogen of the 3rd carrier gas pipe 14 input; surface and neighbouring pollutant are purged clean, forms one layer of nitrogen blanket simultaneously on the surface of VUV discharge lamp；The vaporific extract in ultrasonic atomizatio room 6 is brought into supervisor 12 from the nitrogen of the first carrier gas pipe 1 input, the solvent flashing 9 in solvent flashing storage tank 10 is brought into supervisor 12 from the nitrogen of the second carrier gas pipe 7 input, converge with the extract of gasification, the front end in the port of export arrival atmospheric pressure photoionization source then passing through supervisor 12 is ionized, the ion produced after ionization under the effect of electric field and pressure differential, can enter, by mass spectrometer inlet 16 and mass spectrograph sample feeding pipe 18, the analyzed detection of mass analyzer being in vacuum system.In the positive-ion mode, mass spectrometer inlet 16 being applied with the voltage of-3.5KV, the flow velocity of the dry gas 17 outside mass spectrometric sample feeding pipe 18 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 is mixed for first alcohol and water 3:1 by volume, and solvent flashing 9 is mixed for toluene and methyl phenyl ethers anisole 1:1 by volume；
The port of export of supervisor 12 is perpendicular to mass spectrometer inlet 16, and the spacing of horizontal direction is 15mm between the two, and the spacing of vertical direction is 3mm, VUV discharge lamp 15 to go out light end vertical corresponding up and down with mass spectrometer inlet.
In the positive-ion mode, mass spectrometer inlet 16 being applied with the voltage of-3.5KV, the flow velocity of the dry gas 17 outside mass spectrometric sample feeding pipe 18 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 quickly online atmospheric pressure photoionization mass spectrometer for effective ingredient in complex matrices, including pretreating device, atmospheric pressure photoionization source and mass spectrograph, it is characterised in that:
Described pretreating device includes ultrasonic atomizatio mechanism, solvent flashing retraction mechanism and heat transfer mechanism；
Described ultrasonic atomizatio mechanism includes ultrasound atomizer (3), it is provided with extractant (4) in the ultrasonic atomizatio room (6) of ultrasound atomizer (3), the side of ultrasonic atomizatio room (6) connects the first carrier gas pipe (1), and the first carrier gas pipe (1) is provided with first-class gauge (2)；
Described solvent flashing retraction mechanism includes solvent flashing storage tank (10), is provided with solvent flashing (9) in solvent flashing storage tank (10)；The side of solvent flashing storage tank (10) connects 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)；
Described heat transfer mechanism includes the supervisor (12) keeping steady temperature, the entrance point of described supervisor (12) connects the ultrasonic atomizatio room (6) of ultrasound atomizer (3), the port of export of supervisor (12) correspond to the front end in mass spectrometer inlet (16) and atmospheric pressure photoionization source, and the outlet of solvent flashing storage tank (10) the middle part of supervisor (12)；The temperature of described supervisor (12) remains 200 ~ 500 DEG C；
Determinand (5) is located in the extractant (4) of ultrasonic atomizatio room (6)；
In the positive-ion mode, mass spectrometer inlet (16) being applied with the voltage of-1 ~-6KV, the flow velocity of the dry gas that mass spectrograph sample feeding pipe (18) is outside is at 3 ~ 10L/min, and temperature is at 100 ~ 400 DEG C.
2. according to claim 1 a kind of for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices, 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) goes out light end facing to VUV discharge lamp, and the 3rd carrier gas pipe (14) is provided with the 3rd effusion meter (13).
3. according to claim 1 a kind of for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices, it is characterised 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 Orbitrap mass or tandem mass spectrum.
4. according to claim 1 a kind of for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices, it is characterized in that: being arranged with heater strip (11) on described supervisor (12), the internal diameter of the port of export of supervisor (12) is at 1 ~ 4mm.
5. according to claim 1 a kind of for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices, it is characterized in that: the port of export of described supervisor (12) is 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 described atmospheric pressure photoionization source is perpendicular to the port of export of supervisor (12).
6. according to claim 1 a kind of for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices, it is characterized in that: the port of export of described supervisor (12) is 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 described atmospheric pressure photoionization source is vertical corresponding up and down with mass spectrometer inlet.
7. according to claim 1 a kind of for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices, it is characterised in that: described extractant (4) is mixed for first alcohol and water 3:1 by volume.
8. according to claim 1 a kind of for the quickly online atmospheric pressure photoionization mass spectrometer of effective ingredient in complex matrices, it is characterised in that: described solvent flashing (9) is mixed for toluene and methyl phenyl ethers anisole 1:1 by volume.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620157680.2U CN205404478U (en) | 2016-03-02 | 2016-03-02 | A quick online atmospheric pressure photo ionization mass spectrum device for active ingredient among complicated matrix |
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| CN201620157680.2U CN205404478U (en) | 2016-03-02 | 2016-03-02 | A quick online atmospheric pressure photo ionization mass spectrum device for active ingredient among complicated matrix |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105588872A (en) * | 2016-03-02 | 2016-05-18 | 中国科学技术大学 | Quick on-line atmospheric photo ionization mass spectrum device for effective constituent in complex substrate |
| CN113182108A (en) * | 2021-04-29 | 2021-07-30 | 广州雾普康生物科技有限公司 | Herbal extract atomization method and atomization device |
-
2016
- 2016-03-02 CN CN201620157680.2U patent/CN205404478U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105588872A (en) * | 2016-03-02 | 2016-05-18 | 中国科学技术大学 | Quick on-line atmospheric photo ionization mass spectrum device for effective constituent in complex substrate |
| CN105588872B (en) * | 2016-03-02 | 2018-09-07 | 中国科学技术大学 | A kind of quick online atmospheric pressure photoionization mass spectrometric apparatus for active ingredient in complex matrices |
| CN113182108A (en) * | 2021-04-29 | 2021-07-30 | 广州雾普康生物科技有限公司 | Herbal extract atomization method and atomization device |
| CN113182108B (en) * | 2021-04-29 | 2022-01-28 | 广州雾普康生物科技有限公司 | Herbal extract atomization method and atomization device |
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Granted publication date: 20160727 |
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