CN219625426U - Filtering and enriching detection device - Google Patents
Filtering and enriching detection device Download PDFInfo
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- CN219625426U CN219625426U CN202320867549.5U CN202320867549U CN219625426U CN 219625426 U CN219625426 U CN 219625426U CN 202320867549 U CN202320867549 U CN 202320867549U CN 219625426 U CN219625426 U CN 219625426U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The utility model discloses a filtering and enriching detection device, which comprises a filtering and enriching device and a detection device; the filtration and enrichment device comprises: a multistage filtering device (11), an enrichment diffusion analysis device (12) and an air pump (13); the detection device comprises a single photon ionization time-of-flight mass spectrometer (21) and an orbitrap mass spectrometer. The device of the utility model can accurately measure the content of harmful substances and main components thereof in cigarette aerosol.
Description
Technical Field
The utility model belongs to the technical field of tobacco, and particularly relates to a filtering enrichment detection device.
Background
The components of cigarette aerosol are extremely complex, and generally comprise hydrocarbons, aldehydes, ketones, heterocyclic compounds and other organic matters, carbon dioxide, carbon monoxide, nitrogen oxides and other inorganic gases, particulate matters and other large matters. Up to 5000 kinds of components have been detected from cigarette aerosols, and their kinds and amounts have been increasing over time. Aerosol generated by cigarette combustion can damage respiratory systems of smokers, and becomes one of the primary factors for causing lung cancer and chronic obstructive pulmonary disease. If a great deal of secondhand smoke is inhaled by a human body for a long time, the human body is easy to cause a plurality of discomforts, such as the reduction of immune function, endocrine dyscrasia and the like.
The compound in the coil smoke sol has certain specificity and small sample flux, and the detection technology is required to have the characteristics of high sensitivity and high selectivity. Conventional detection and analysis technologies of the existing cigarette aerosol include chromatography, mass spectrometry and the like. Among them, gas chromatography and liquid chromatography-mass spectrometry are two methods commonly used for detecting compounds in aerosols. However, because the detected aerosol sample has complex components and low concentration content, the aerosol sample is often required to be combined with other pretreatment methods in the process of performing instrument detection analysis on the sample so as to completely extract components in the aerosol as much as possible, thereby improving the sensitivity of the method. Common pretreatment methods include liquid-liquid extraction, solid-phase microextraction and the like, but the methods generally have the defects of complicated operation steps and long time consumption, and are difficult to realize rapid analysis of samples.
In the analysis of aerosol components of cigarettes, researchers are currently focusing on the measurement of the particle size distribution of organic compounds, inorganic substances or particulate matter alone, without a device capable of uniformly and effectively analyzing all aerosol components. The single photon ionization mass spectrum is an on-line monitoring technology of volatile organic compounds based on the photoionization technology, and the technology has the advantages of broad-spectrum soft ionization, less fragment peaks, high sensitivity and short response time, and can be used for real-time on-line detection of complex samples. However, at present, no device for processing aerosol at the front end of a real-time online single photon ionization mass spectrum sample injection system exists, and the device can collect, transmit and filter the aerosol generated by natural combustion of cigarettes, so that a rapid, accurate and effective method is provided for accurately measuring the content of harmful substances and main components thereof in the cigarette aerosol. Meanwhile, the single photon ionization mass spectrum can only carry out ionization detection analysis on volatile organic compounds with ionization energy smaller than 10.6eV, and the components in the cigarette aerosol reach more than 5000, so that the components in the cigarette aerosol can not be completely detected by using the single photon ionization mass spectrum, and detection needs to be carried out by combining other instruments.
The utility model is proposed for this purpose.
Disclosure of Invention
The utility model discloses a filtering enrichment detection device and a detection method for coiled smoke sol. The device adopts a multi-layer membrane filter device to collect, transmit, filter and sample the cigarette aerosol generated by the natural burning of the cigarettes.
The technical scheme of the utility model is as follows:
the first aspect of the utility model discloses a filtering and enriching detection device, which comprises a filtering and enriching device and a detection device;
the filtration and enrichment device comprises: a multistage filtering device 11, an enrichment diffusion analysis device 12 and an air pump 13;
the detection means comprises a single photon ionization time-of-flight mass spectrometer 21 and an orbitrap mass spectrometer.
Preferably, the multistage filtration device 11 is a plurality of filtration membrane devices connected in series, each filtration membrane device comprises a sheet membrane 111, a membrane support net 112, an O-shaped rubber ring 113 and a sealing fixing plate 114; each filtering membrane device is provided with an air inlet and an air outlet in a sealing way; the film supporting net 112 is formed by sequentially laminating a plurality of sheet film supporting nets, and can be used for placing one, two and a plurality of sheet films 111 to be freely combined according to the requirement; the modular design can facilitate the replacement of damaged particle filtration membranes; the membrane supporting net 112 can increase the pressure difference born by the sheet membrane 111, so as to avoid the damage of the sheet membrane 111; a sealed O-shaped rubber ring 113 is arranged on the sheet membrane 111, and the upper part of the sealed O-shaped rubber ring 113 is buckled and sealed; the multi-stage membrane structure can be established according to actual conditions, and can be one-stage, two-stage or even more stages.
Preferably, the air inlet of the first filtering membrane device of the plurality of filtering membrane devices connected in series is an aerosol inlet 3 for an aerosol inlet of a cigarette sample 4, a carrier gas inlet 31 is arranged on the side wall of the aerosol inlet 3, the carrier gas is helium or nitrogen, the carrier gas carries sample gas to the surface of the sheet membrane 111, finally, the sample gas is diffused into a mass spectrum sample inlet for analysis after passing through the sheet membrane 111, and the redundant sample gas is pumped and discharged through an aerosol outlet and a sucking pump 13; the gas outlet of the last filtering membrane device of the plurality of filtering membrane devices connected in series is connected with the enrichment diffusion analysis device 12, one end of the enrichment diffusion analysis device 12 is connected with the air pump 13, and the other end of the enrichment diffusion analysis device is connected with the single photon ionization time-of-flight mass spectrometer 21.
Preferably, the enrichment diffusion analysis device 12 comprises an organic semipermeable membrane under vacuum; the organic semipermeable membrane is one of a polydimethylsiloxane membrane (PDMS), a polytetrafluoroethylene membrane, a cellulose membrane or a polyethylene membrane, and can be selected according to target molecules; the film thickness is generally 0.05mm.
Preferably, the pore diameter of the sheet film 111 is 0.01 to 10.0 μm, and the thickness is 20 to 300 μm; the sheet-shaped film 111 is made of glass fiber, polytetrafluoroethylene, or other self-made composite fiber films, or other commercial films; the flaky membrane can sequentially filter 10 μm, 1 μm, 0.1 μm and 0.01 μm ultrafine particles.
Preferably, the carrier gas is helium, nitrogen or a mixture of the two, and other inert gases may be used.
Preferably, the flow rate of the air pump 13 is 30 mL/min-40 mL/min.
The utility model discloses a detection method of cigarette aerosol in a second aspect, which uses the device and comprises the following steps:
starting the air extracting pump 13; igniting the cigarette sample 4, and enabling generated aerosol to enter through the aerosol inlet 3 and simultaneously introducing carrier gas from the carrier gas inlet 31; the mixed gas of aerosol and carrier gas enters a filtering membrane device, is filtered by a plurality of filtering membrane devices, is enriched by an organic semi-permeable membrane in an enrichment diffusion analysis device 12, and enters a single photon ionization time-of-flight mass spectrometer 21 for analysis after diffusion and analysis; the redundant sample gas aerosol and carrier gas mixed gas is pumped and discharged through a sucking pump; the ionization source of the single photon ionization time-of-flight mass spectrometer 21 adopts a vacuum ultraviolet krypton lamp, and the single photon energy is 10.6eV; the analyzer adopts a vertical-lead reflective time-of-flight mass analyzer; the single photon ionization time-of-flight mass spectrometer 21 samples: the injection process of the organic semipermeable membrane such as PDMS membrane is divided into three steps: enrichment, diffusion and analysis; 1. the PDMS film is used for selectively enriching the sample to be detected; 2. forming a concentration gradient diffusion film by the sample to be tested; 3. analyzing and desorbing the sample to be tested on the high vacuum side under the action of pressure difference; the PDMS film has a certain enrichment effect on sample molecules, and can ensure higher sensitivity of the mass spectrometer to a certain extent (generally tens to hundreds times of that of an injection sample mode); in the diffusion process, different sample molecules have different solubilities in the membrane, and under the action of pressure difference at two sides of the membrane, a sample with high solubility is enriched at a high vacuum side and then enters a mass spectrum for ionization detection analysis.
The organic compound enriched on the sheet-like film 111 was eluted using an organic solvent, and the eluent was measured using an orbitrap mass spectrometer to qualitatively determine the kind of the organic compound in the eluent.
Preferably, the organic solvent is methanol, acetonitrile or a mixture of the methanol and the acetonitrile, and the eluent is filtered by using a filter membrane with a filter hole of 0.22 mu m; ultrasonically extracting the enriched sheet-like membrane 111 with a certain amount of organic solvent such as methanol/acetonitrile for several times, and mixing the extracts; blowing nitrogen to near dryness, adding organic solvent to dissolve residue, mixing for 1min by vortex, filtering with 0.22 μm filter membrane, and measuring the filtered eluate with orbitrap mass spectrometer.
The utility model has the beneficial effects that:
the utility model discloses a filtering enrichment detection device, which combines the operation conditions of a real-time online single photon ionization mass spectrometer to design a multi-stage membrane device capable of collecting, transmitting and filtering aerosol generated by natural combustion of cigarettes. The device effectively solves the problem of residual film sample injection device of a single photon ionization mass spectrometer caused by the too high concentration of the particles in the cigarette aerosol; meanwhile, the organic solvent is used for eluting the flaky membrane of the device, and the detection is carried out by combining an orbitrap mass spectrometer, so that the qualitative analysis of the organic compounds in the cigarette aerosol can be carried out. To accurately measure the content of the aerosol in the cigarettesThe content of the harmful substances and the main components thereof provides a rapid, accurate and effective method. The filtering enrichment detection device introduces N into a multistage membrane device 2 /He；N 2 He is not only carrier gas, but also aerosol is diluted to a certain extent when the aerosol is put into the sample injection end of the single photon ionization mass spectrometer; meanwhile, the aerosol passes through the surface of the multistage membrane, so that the membrane also enriches the components in the aerosol, and also plays a role in dilution to ppb level.
Drawings
FIG. 1 is a schematic diagram of a filtration-enrichment detection device of the present utility model.
FIG. 2 is a schematic diagram of a single filtration membrane device.
Fig. 3 is a workflow diagram of a method of detecting cigarette aerosols using the apparatus of the utility model.
FIG. 4 is a graph showing the results of the detection of a coil aerosol using the apparatus of the present utility model.
The reference numerals are: 11. a filtering device; 111. a sheet-like film; 112. a membrane support net; 113. an O-shaped rubber ring; 114. sealing the fixing plate; 12. enrichment diffusion analysis device; 13. an air extracting pump; 21. a single photon ionization time-of-flight mass spectrometer; 3. an aerosol inlet; 4. and (5) a cigarette sample.
Detailed Description
The present utility model will be described in further detail by the following specific embodiments, but it should not be construed that the scope of the present utility model is limited to the following examples. Various substitutions and alterations are also within the scope of this disclosure, as will be apparent to those of ordinary skill in the art and by routine experimentation, without departing from the spirit of the utility model as defined by the foregoing description.
As shown in FIG. 1, the utility model discloses a filtering and enriching detection device, which comprises a filtering and enriching device and a detection device; the filtration and enrichment device comprises: a multistage filtering device 11, an enrichment diffusion analysis device 12 and an air pump 13; the detection means include a single photon ionization time-of-flight mass spectrometer 21 and an orbitrap mass spectrometer (not shown). The multistage filtering device 11 is a plurality of filtering membrane devices connected in series, and each filtering membrane device comprises a sheet membrane 111, a membrane supporting net 112, an O-shaped rubber ring 113 and a sealing fixing plate 114; each filtering membrane device is provided with an air inlet and an air outlet in a sealing way; the film supporting net 112 is formed by sequentially laminating a plurality of sheet film supporting nets, and can be used for placing one, two and a plurality of sheet films 111 to be freely combined according to the requirement; the modular design can facilitate the replacement of damaged particle filtration membranes; the membrane supporting net 112 can increase the pressure difference born by the sheet membrane 111, so as to avoid the damage of the sheet membrane 111; a sealed O-shaped rubber ring 113 is arranged on the sheet membrane 111, and the upper part of the sealed O-shaped rubber ring 113 is buckled and sealed; the multi-stage membrane structure can be established according to actual conditions, and can be one-stage, two-stage or even more stages. The utility model provides three filtering membrane devices, each of which has a sheet membrane 111 therein.
The gas inlet of the first filtering membrane device of the plurality of filtering membrane devices connected in series is an aerosol inlet 3 for a cigarette sample 4, a carrier gas inlet 31 is arranged on the side wall of the aerosol inlet 3, the carrier gas is helium or nitrogen, the carrier gas carries sample gas to the surface of the sheet membrane 111, finally the sample gas is diffused into a mass spectrum sample inlet for analysis after passing through the sheet membrane 111, and redundant sample gas is discharged after being pumped through an aerosol outlet through a suction pump; the gas outlet of the last filtering membrane device of the plurality of filtering membrane devices connected in series is connected with the enrichment diffusion analysis device 12, one end of the enrichment diffusion analysis device 12 is connected with the air pump 13, and the other end of the enrichment diffusion analysis device is connected with the single photon ionization time-of-flight mass spectrometer 21. The filtering and detecting device for the coiled smoke sol introduces N into a multistage membrane device 2 /He；N 2 He is not only carrier gas, but also dilution of aerosol to a certain extent when the cigarette aerosol is put into the sample injection end of the single photon ionization mass spectrometer; meanwhile, the coiled smoke sol passes through the surface of the multistage membrane, so that the membrane also enriches the components in the aerosol, and also plays a role in dilution to ppb level.
Wherein the enrichment diffusion analysis device 12 comprises an organic semi-permeable membrane in a vacuum state; the organic semipermeable membrane is one of a polydimethylsiloxane membrane (PDMS), a polytetrafluoroethylene membrane, a cellulose membrane or a polyethylene membrane, and can be selected according to the condition of target molecules; the film thickness is generally 0.05mm. According to the utility model, a PDMS film with a film thickness of 0.05mm is selected as an organic semipermeable film.
Wherein the pore diameter of the sheet film 111 is 0.01-10.0 μm, and the thickness is 20-300 μm; the sheet-shaped film 111 is made of glass fiber, polytetrafluoroethylene, or other self-made composite fiber films, or other commercial films; the flaky membrane can sequentially filter 10 μm, 1 μm, 0.1 μm and 0.01 μm ultrafine particles. The polytetrafluoroethylene film is selected as a sheet-shaped film 111, and the pore diameters are 10 mu m, 1 mu m, 0.1 mu m and 0.01 mu m, and the thicknesses are 100 mu m respectively.
Wherein, the flow rate of the air pump 13 is 30 mL/min-40 mL/min.
The method for detecting the cigarette aerosol by using the filtering and enriching detection device comprises the following steps:
starting the air extracting pump 13; igniting the cigarette sample 4, and enabling generated aerosol to enter through the aerosol inlet 3 and simultaneously introducing carrier gas from the carrier gas inlet 31; the mixed gas of aerosol and carrier gas enters a filtering membrane device, is filtered by a plurality of filtering membrane devices, is enriched by an organic semi-permeable membrane in an enrichment diffusion analysis device 12, and enters a single photon ionization time-of-flight mass spectrometer 21 for analysis after diffusion and analysis; the redundant sample aerosol and carrier gas mixture is pumped and discharged by an air pump; the ionization source of the single photon ionization time-of-flight mass spectrometer 21 adopts a vacuum ultraviolet krypton lamp, and the single photon energy is 10.6eV; the analyzer adopts a vertical-lead reflective time-of-flight mass analyzer; the single photon ionization time-of-flight mass spectrometer 21 samples: the injection process of the organic semipermeable membrane such as PDMS membrane is divided into three steps: enrichment, diffusion and analysis; firstly, selectively enriching a sample to be detected by a PDMS film; secondly, forming a concentration gradient diffusion film on the sample to be detected; thirdly, analyzing and desorbing the sample to be tested on the high vacuum side under the action of the pressure difference; the PDMS film has a certain enrichment effect on sample molecules, and can ensure higher sensitivity of the mass spectrometer to a certain extent (generally tens to hundreds times of that of an injection sample mode); in the diffusion process, different sample molecules have different solubilities in the membrane, and under the action of pressure difference at two sides of the membrane, a sample with high solubility is enriched at a high vacuum side and then enters a mass spectrum for ionization detection analysis.
The organic compound enriched on the sheet-like film 111 was eluted using an organic solvent, and the eluent was measured using an orbitrap mass spectrometer to qualitatively determine the kind of the organic compound in the eluent. The orbitrap mass spectrometer is not shown in the drawings.
Wherein the organic solvent is methanol, acetonitrile or a mixture of the methanol and the acetonitrile, and the eluent is filtered by a filter membrane with a filter hole of 0.22 mu m; ultrasonically extracting the enriched sheet-like membrane 111 with a certain amount of organic solvent such as methanol/acetonitrile for several times, and mixing the extracts; blowing nitrogen to near dryness, adding organic solvent to dissolve residue, mixing for 1min by vortex, filtering with 0.22 μm filter membrane, and measuring the filtered eluate with orbitrap mass spectrometer.
The device provided by the utility model can be combined with a real-time online single photon ionization mass spectrometer and an orbitrap mass spectrometer to accurately measure the content of harmful substances and main components thereof in cigarette aerosol. The results are shown in FIG. 4.
The examples are given solely for the preferred embodiments of the present utility model and are not intended to limit the utility model thereto, since various modifications and variations will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present utility model should be included in the protection scope of the present utility model.
Claims (5)
1. The filtering and enriching detection device is characterized by comprising a filtering and enriching device and a detection device;
the filtration and enrichment device comprises: a multistage filtering device (11), an enrichment diffusion analysis device (12) and an air pump (13);
the detection device comprises a single photon ionization time-of-flight mass spectrometer (21) and an orbitrap mass spectrometer.
2. The device according to claim 1, characterized in that the multi-stage filtration device (11) is a plurality of filtration membrane devices connected in series, each filtration membrane device comprising a sheet membrane (111), a membrane support mesh (112), an O-ring rubber (113) and a sealing fixation plate (114); each filtering membrane device is provided with an air inlet and an air outlet in a sealing way.
3. The device according to claim 2, characterized in that the air inlet of the first filter membrane device of the plurality of filter membrane devices connected in series is an aerosol inlet (3) for a cigarette sample (4), a carrier gas inlet (31) being provided on the side wall of the aerosol inlet (3); the gas outlet of the last filtering membrane device of the plurality of filtering membrane devices connected in series is connected with the enrichment diffusion analysis device (12), one end of the enrichment diffusion analysis device (12) is connected with the sucking pump (13), and the other end of the enrichment diffusion analysis device is connected with the single photon ionization time-of-flight mass spectrometer (21).
4. A device according to claim 3, characterized in that the enriched diffusion resolution means (12) comprise an organic semi-permeable membrane in a vacuum state; the organic semipermeable membrane is one of a polydimethylsiloxane membrane, a polytetrafluoroethylene membrane, a cellulose membrane or a polyethylene membrane.
5. The device according to claim 2, characterized in that the sheet-like membrane (111) has a pore size of 0.01-10.0 μm and a thickness of 20-300 μm; the sheet-like film (111) is made of glass fiber or polytetrafluoroethylene.
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| CN202320867549.5U CN219625426U (en) | 2023-04-18 | 2023-04-18 | Filtering and enriching detection device |
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| CN202320867549.5U CN219625426U (en) | 2023-04-18 | 2023-04-18 | Filtering and enriching detection device |
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