CN115808462B - Method for eliminating ammonia gas signal and/or volatile organic amine in ion mobility spectrometry and method for detecting sample - Google Patents
Method for eliminating ammonia gas signal and/or volatile organic amine in ion mobility spectrometry and method for detecting sample Download PDFInfo
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- CN115808462B CN115808462B CN202211621694.1A CN202211621694A CN115808462B CN 115808462 B CN115808462 B CN 115808462B CN 202211621694 A CN202211621694 A CN 202211621694A CN 115808462 B CN115808462 B CN 115808462B
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- volatile organic
- mobility spectrometry
- ammonia
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 185
- 150000001412 amines Chemical class 0.000 title claims abstract description 87
- 238000001871 ion mobility spectroscopy Methods 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 78
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 15
- 239000000523 sample Substances 0.000 claims description 110
- 150000002500 ions Chemical class 0.000 claims description 29
- 210000002700 urine Anatomy 0.000 claims description 17
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims description 16
- 239000012472 biological sample Substances 0.000 claims description 15
- 239000002841 Lewis acid Substances 0.000 claims description 11
- 150000007517 lewis acids Chemical class 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 235000003704 aspartic acid Nutrition 0.000 claims description 9
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims description 9
- 239000008280 blood Substances 0.000 claims description 9
- 210000004369 blood Anatomy 0.000 claims description 9
- 238000001228 spectrum Methods 0.000 claims description 9
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- 150000003839 salts Chemical class 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- 150000007522 mineralic acids Chemical class 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- ZSUXOVNWDZTCFN-UHFFFAOYSA-L tin(ii) bromide Chemical compound Br[Sn]Br ZSUXOVNWDZTCFN-UHFFFAOYSA-L 0.000 claims description 6
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 claims description 6
- 235000013305 food Nutrition 0.000 claims description 5
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 4
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims description 4
- 241001465754 Metazoa Species 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- KPWJBEFBFLRCLH-UHFFFAOYSA-L cadmium bromide Chemical compound Br[Cd]Br KPWJBEFBFLRCLH-UHFFFAOYSA-L 0.000 claims description 4
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 4
- 239000004220 glutamic acid Substances 0.000 claims description 4
- 235000013922 glutamic acid Nutrition 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 235000011150 stannous chloride Nutrition 0.000 claims description 4
- 239000001119 stannous chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical compound I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 claims description 4
- UCYRAEIHXSVXPV-UHFFFAOYSA-K bis(trifluoromethylsulfonyloxy)indiganyl trifluoromethanesulfonate Chemical compound [In+3].[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F.[O-]S(=O)(=O)C(F)(F)F UCYRAEIHXSVXPV-UHFFFAOYSA-K 0.000 claims description 3
- 150000001649 bromium compounds Chemical class 0.000 claims description 3
- 150000001805 chlorine compounds Chemical class 0.000 claims description 3
- 150000004820 halides Chemical class 0.000 claims description 3
- VRDNAHLDDUCBMP-UHFFFAOYSA-K indium(3+);2,2,2-trifluoroacetate Chemical compound [In+3].[O-]C(=O)C(F)(F)F.[O-]C(=O)C(F)(F)F.[O-]C(=O)C(F)(F)F VRDNAHLDDUCBMP-UHFFFAOYSA-K 0.000 claims description 3
- 235000013622 meat product Nutrition 0.000 claims description 3
- 229960002523 mercuric chloride Drugs 0.000 claims description 3
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical group Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 210000003296 saliva Anatomy 0.000 claims description 3
- 229940102001 zinc bromide Drugs 0.000 claims description 3
- VCQWRGCXUWPSGY-UHFFFAOYSA-L zinc;2,2,2-trifluoroacetate Chemical compound [Zn+2].[O-]C(=O)C(F)(F)F.[O-]C(=O)C(F)(F)F VCQWRGCXUWPSGY-UHFFFAOYSA-L 0.000 claims description 3
- YXTDAZMTQFUZHK-ZVGUSBNCSA-L (2r,3r)-2,3-dihydroxybutanedioate;tin(2+) Chemical compound [Sn+2].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O YXTDAZMTQFUZHK-ZVGUSBNCSA-L 0.000 claims description 2
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 210000000941 bile Anatomy 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- RJYMRRJVDRJMJW-UHFFFAOYSA-L dibromomanganese Chemical compound Br[Mn]Br RJYMRRJVDRJMJW-UHFFFAOYSA-L 0.000 claims description 2
- 238000000766 differential mobility spectroscopy Methods 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- 210000004209 hair Anatomy 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 210000002966 serum Anatomy 0.000 claims description 2
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 2
- 229940007163 stannous tartrate Drugs 0.000 claims description 2
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 2
- 210000001835 viscera Anatomy 0.000 claims description 2
- NGJQIQUNRRHCHB-UHFFFAOYSA-N CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.OC(=O)C(O)=O Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.OC(=O)C(O)=O NGJQIQUNRRHCHB-UHFFFAOYSA-N 0.000 claims 1
- 238000004949 mass spectrometry Methods 0.000 claims 1
- 229960001939 zinc chloride Drugs 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 16
- 230000008030 elimination Effects 0.000 abstract description 11
- 238000003379 elimination reaction Methods 0.000 abstract description 11
- 230000005764 inhibitory process Effects 0.000 abstract description 4
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- 239000007789 gas Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 235000001014 amino acid Nutrition 0.000 description 6
- 150000001413 amino acids Chemical class 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 5
- 239000013043 chemical agent Substances 0.000 description 5
- 230000005012 migration Effects 0.000 description 5
- 238000013508 migration Methods 0.000 description 5
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical group CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 4
- 239000012491 analyte Substances 0.000 description 4
- 230000012447 hatching Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
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- 239000000243 solution Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 description 2
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
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- 238000007086 side reaction Methods 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- MXSVLWZRHLXFKH-UHFFFAOYSA-N triphenylborane Chemical compound C1=CC=CC=C1B(C=1C=CC=CC=1)C1=CC=CC=C1 MXSVLWZRHLXFKH-UHFFFAOYSA-N 0.000 description 2
- 241000272525 Anas platyrhynchos Species 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
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- 102100031948 Enhancer of polycomb homolog 1 Human genes 0.000 description 1
- 102100031941 Enhancer of polycomb homolog 2 Human genes 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
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- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
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- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000000370 acceptor Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- -1 ammonium ions Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
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- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
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- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
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- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 230000007274 generation of a signal involved in cell-cell signaling Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
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- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
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- KHPXUQMNIQBQEV-UHFFFAOYSA-N oxaloacetic acid Chemical compound OC(=O)CC(=O)C(O)=O KHPXUQMNIQBQEV-UHFFFAOYSA-N 0.000 description 1
- 235000015277 pork Nutrition 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
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- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
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- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 238000013055 trapped ion mobility spectrometry Methods 0.000 description 1
- 229910052722 tritium Inorganic materials 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a method for eliminating ammonia gas signals and/or volatile organic amines in an ion mobility spectrometry and a method for detecting a sample, and relates to the technical field of ion mobility spectrometry analysis and detection. The elimination method comprises the step of treating a sample to be tested with a chemical reagent. And fixing a large amount of ammonia gas and/or volatile organic amine in the sample to be tested by a chemical method to form a stable compound so as to prevent the ammonia gas or volatile organic amine from volatilizing out and entering and polluting an ion mobility spectrometry system. The validity and the easy analysis of the sample acquisition data are ensured, and the detection efficiency is greatly improved. The invention provides a new thought aiming at sample ammonia or volatile organic amine signal inhibition, and the scientificity and effectiveness of the thought are verified through the trial of various reagents.
Description
Technical Field
The invention relates to the technical field of ion mobility spectrometry analysis and detection, in particular to a method for eliminating ammonia gas signals and/or volatile organic amines in ion mobility spectrometry and a method for detecting samples.
Background
Gas phase ion mobility spectrometry (GC-IMS) is a combined technique of Gas Chromatography (GC) and Ion Mobility Spectrometry (IMS). For detecting trace amounts of volatile substances, chromatography is responsible for separating complex components, and ion mobility spectrometry can be used as a detector for chromatography. Ion migration occurs in an ion migration tube and is divided into two processes, namely ionization, namely that molecules of an object to be detected are charged with certain charges, and migration, namely that the ionized molecules of the object to be detected move under the action of an electric field. The ion transfer tube structure is shown in fig. 1.
Tritium source (T, beta ray) is one of common ionization sources of civil GC-IMS, and beta electron energy is small, so that chemical bonds cannot be directly broken, and fragment ions are generated. Under beta-ray irradiation, nitrogen (GC carrier gas) and trace amounts of water contained in the nitrogen undergo a series of chemical processes to finally form hydrated protons H +(H2O)n, also called reactive ions. The reaction ion transfers hydrogen proton (H +) to the molecule of the object to be detected through the proton transfer process, so that the molecule of the object to be detected has a unit positive charge, H +(H2O)n becomes neutral water molecule, and the molecule of the object to be detected completes ionization, namely the process of chemical ionization. Finally, the charged molecules of the object to be detected can be migrated under the action of the electric field and reach the detector to be detected. Therefore, the process of proton transfer of the hydrated proton H +(H2O)n to the molecule of the object to be detected to form the molecular ion (H + M) of the object to be detected is the most basic precondition of Ion Mobility Spectrometry (IMS) detection.
Generally, the process of detecting biological samples is shown in fig. 2, and mainly comprises the steps of firstly filling a liquid or solid biological sample into a gas-phase headspace bottle, sealing the gas-phase headspace bottle by a bottle cap, heating, vibrating and incubating for a period of time, and then extracting a certain volume of headspace gas for sample injection detection to obtain information of volatile substance components in the biological sample.
The biological sample generally contains a large amount of ammonia components and/or volatile organic amines (relative to other volatile components), which can affect data acquisition of GC-IMS, increase difficulty in data analysis, and even cause data failure. Meanwhile, a large amount of ammonia gas and/or volatile organic amine also pollute a GC-IMS system, is not easy to clean, and greatly influences experimental efficiency. Inhibition of ammonia and/or volatile organic amines in a particular sample is highly desirable.
The gas phase ion mobility spectrometry generally uses high-purity nitrogen (99.999%) as a carrier gas, and the carrier gas (the carrier gas contains trace water molecules) always flows through the whole GC-IMS system at a certain flow rate, so that the formation of hydrated protons H +(H2O)n is continuous, and in the spectrogram of the GC-IMS, a signal peak of H +(H2O)n can be always observed, as shown by an arrow of fig. 3, a "vertical line", and a strip signal, namely, a signal peak of H +(H2O)n (also called as a reactive ion peak, reactant Iron Peak, abbreviated as RIP peak). Within the dashed box is the signal of the molecules of the analyte ionized by the proton transfer process.
Since the biological sample such as urine, saliva, blood and the like generally contains a large amount of ammonia components and/or volatile organic amines, the ammonia components and/or volatile organic amines are easy to remain and accumulate in the chromatographic column, and the chromatographic column cannot effectively separate, so that the ammonia components and/or volatile organic amines are continuously eluted with the components to be tested into the migration tube, that is, a large amount of 'impurity' cations exist in the ion migration tube, as shown in two vertical lines at a yellow short line of fig. 4, and are parallel to a hydrated proton peak (RIP peak), and the strength is high. The presence of a large number of "impurity" cations can affect the normal proton transfer of other analyte molecules, thereby affecting the qualitative and quantitative properties of the analyte molecules. As shown in FIG. 4, when ammonia tailing is severe, a strip signal similar to RIP peak is formed, and at this time, the analyte undergoes other side reactions in addition to the proton transfer process normal to the hydrated protons. On the corresponding spectrogram, a plurality of signals can appear in one object molecule to be detected, as shown in a dashed line frame, the signal on the left side in the frame is a normal signal of the object molecule to be detected, the signal on the right side in the frame is a miscellaneous peak appearing in the side reaction process, and the intensity of the miscellaneous peak depends on the content of ammonia in a sample and the residue in a chromatographic column, so that the complexity of the spectrogram is increased and becomes uncontrollable. Even after the ammonia content reaches a certain level. The normal signal of the molecule of the object to be detected disappears, which greatly influences the qualitative and quantitative properties of each component, so that the obtained spectrogram and data fail.
In addition, the residual ammonia in the chromatographic column can be increased along with the detection, and the ammonia is difficult to elute after the detection, so that the influence of ammonia signals becomes unacceptable after the detection of a certain amount of biological samples, thorough cleaning is required, and the detection efficiency is greatly influenced.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a method for eliminating ammonia gas signals and/or volatile organic amines in ion mobility spectrometry and a method for detecting samples so as to prevent the influence of the ammonia gas signals on other substances.
The impact of ammonia signaling on biological sample detection is severe and must be addressed. Firstly because its effect is not controllable and secondly because its accumulation necessarily aggravates its effect, which can lead to the collected spectra not accurately describing the composition of the volatile substances in the sample, leading to erroneous conclusions. The key to solving the problem is how to prevent or partially prevent the influence of ammonia signaling on other substances. The inventors have found that the best way to eliminate the effect of ammonia on detection is to prevent ammonia from entering the ion mobility spectrometry system, e.g. for gas phase ion mobility spectrometry (GC-IMS) systems. Not only avoiding the residue and accumulation in the chromatographic column, but also thoroughly avoiding the signal of ammonia. And aiming at gas phase ion mobility spectrometry, the signal of ammonia gas can be avoided.
The invention is realized in the following way:
The invention provides a method for eliminating ammonia gas signals and/or volatile organic amine in ion mobility spectrometry, and treating the sample to be tested with a chemical reagent to chemically fix ammonia and/or volatile organic amine in the sample to be tested.
The inventor finds that ammonia gas and/or volatile organic amine in the biological sample are fixed through a certain reaction, so that the ammonia gas cannot volatilize and is sucked by a sample injection needle and injected. The ammonia molecules themselves readily combine with hydrogen protons to form ammonium ions (NH 4 +), so ammonia becomes alkaline after dissolution in water, which is the result of ammonia hydrolysis. The ammonium ion is a soluble cation, and is stable under acidic conditions and is dissolved in water in an ionic form, so that the ammonium ion is not volatilized. By adjusting the pH value of the sample to be tested, volatilization of ammonia can be effectively inhibited.
The inventors have immobilized ammonia and/or volatile organic amines by specific chemical processes to avoid volatilizing to the headspace and entering an ion mobility spectrometry system (e.g., GC-IMS system). The ammonia and/or the volatile organic amine have lone pair electrons, can be used as electron donors, and belong to alkaline compounds according to Lewis acid-base theory, so that chemical reagents can be used as electron acceptors to be combined with the ammonia, and the ammonia and/or the volatile organic amine are fixed to avoid volatilization. The volatile organic amine is selected, for example, from triethylamine, trimethylamine, ethylenediamine.
In a preferred embodiment of the present invention, the chemical agent is at least one selected from the group consisting of a non-volatile inorganic acid or a salt thereof, a non-volatile organic acid or a salt thereof, and a Lewis acid.
The inventors have found that the degree of acidity has a certain effect on the elimination of ammonia and/or volatile organic amine signals.
Under the condition that the acidity is as strong as possible, the elimination effect of ammonia and/or volatile organic amine signals is better. The weak acid chemical reagent can also eliminate ammonia and/or volatile organic amine signals to a certain extent, so long as the effect of eliminating ammonia and/or volatile organic amine signals to a certain extent is within the protection scope of the invention.
The selected acid can not volatilize itself, can not influence the volatilization of other substances, and can not destroy the components of other substances.
In an alternative embodiment, the non-volatile inorganic acid is selected from nitric acid, sulfuric acid, or phosphoric acid;
In an alternative embodiment, the non-volatile organic acid is selected from aspartic acid or glutamic acid.
For example aspartic acid (Asp), isoelectric point pi=2.97.
The salt of the non-volatile inorganic acid is selected from silver nitrate.
The salt of the non-volatile organic acid is selected from the group consisting of oxaloacetate.
In an alternative embodiment, the Lewis acid is selected from the group consisting of ions, halides, or Al (CH 3)3;
In an alternative embodiment, the Lewis acid is selected from Cr ion, hg ion, co ion, cu ion, au ion, ag ion, or Pd ion. The effect of Ag is better than Hg.
For example, the Lewis acid is selected from Cr 3+、Hg2+、Co3+、Cu+、Cu2+、Au3+、Ag+、Pd2+.
In an alternative embodiment, the Lewis acid is selected from the group consisting of zinc chloride, zinc bromide, zinc iodide, manganese chloride, manganese bromide, cadmium chloride, cadmium bromide, stannous chloride, stannous bromide, stannous sulfate, stannous tartrate, indium trifluoromethylsulfonate, indium trifluoroacetate, zinc trifluoroacetate, chlorides or bromides of rare earth elements, cobalt chloride, ferrous chloride, yttrium chloride, aluminum chloride, and mixtures thereof.
In an alternative embodiment, examples of Lewis acids include chlorides or bromides of rare earth elements such as lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, hafnium, erbium, thallium, ytterbium, and lutetium.
Organometallic compounds such as triphenylborane, titanium isopropoxide can also be used as Lewis acids.
In an alternative embodiment, a mixture of two or more Lewis acids may of course be used.
Among the Lewis acids, for example, one selected from zinc chloride, zinc bromide, stannous chloride, stannous bromide, triphenylborane and zinc chloride/stannous chloride mixtures, indium triflate, indium trifluoroacetate and zinc trifluoroacetate.
In a preferred embodiment of the present invention, the sample to be tested is a sample with ammonia component.
In an alternative embodiment, the sample to be tested is a biological sample or a food sample with an ammonia component.
In an alternative embodiment, the biological sample is urine, saliva, blood, serum or bile.
In an alternative embodiment, the food sample is selected from the group consisting of tea leaves, meat products, aquatic products, fermented products, and animal tissue, e.g., animal tissue is selected from the group consisting of animal fur or viscera.
Meat products include, but are not limited to, beef, pork, mutton, fish, shrimp, rabbit, chicken, duck.
In a preferred embodiment of the present invention, the method of elimination includes mixing the sample to be tested with a chemical agent, wherein the mass of the chemical agent is 0.1% -50% of the mass of the sample to be tested (e.g., solid sample). For example 5% -15%,5% -10%,6% -15%,8% -12%,1% -45%. In other embodiments, the mass of the chemical agent exceeds 50% of the mass of the sample to be tested.
When the sample is in a liquid state, the measurement is performed in a volume mode, and the sample adding amount (mass or volume) of the liquid sample accounts for 0.1% -50% of the mass of the sample to be measured (such as a solid sample).
After mixing, if the chemical is in excess, a solid precipitate of chemical (e.g., amino acid) can be observed at the bottom of the bottle. In an alternative embodiment, the amount of chemical agent added may be set to be excessive or excessive, as desired.
The invention also provides a method for detecting the sample by adopting the ion mobility spectrometry, which comprises the following steps of fixing the ammonia gas and/or the volatile organic amine in the sample by adopting the method for eliminating the ammonia gas and/or the volatile organic amine signal and/or the volatile organic amine in the ion mobility spectrometry, then heating and hatching a sealed container filled with the sample to be detected, and taking the top air to enter the ion mobility spectrometry for detection.
In a preferred embodiment of the present invention, the above-mentioned heat hatching is performed by placing the sealed container at a temperature of 40-120 ℃.
Such as 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃, or 120 ℃.
In an alternative embodiment, hatching is performed at 60-120 ℃ when the sample to be tested is a biological sample.
In an alternative embodiment, hatching is performed at 40-100 ℃ when the sample to be tested is a food sample.
In a preferred embodiment of the invention, the incubation time is 2-20min. For example 2-8min,5-10min.
In a preferred embodiment of the invention, the single needle analysis time is 5-40min during detection. The single needle analysis time is 15-18min,15-19min.
In a preferred embodiment of the invention, the ion mobility spectrometry is drift time ion mobility spectrometry, inhalation ion mobility spectrometry, traveling wave ion mobility spectrometry, high-field asymmetric waveform ion mobility spectrometry, and trapped ion mobility spectrometry.
In a preferred embodiment of the invention, the ion mobility spectrometry is gas phase ion mobility spectrometry.
The invention has the following beneficial effects:
According to the invention, a large amount of ammonia gas and/or volatile organic amine in a sample to be detected is fixed by a chemical method to form a stable compound so as to prevent the ammonia gas and/or the organic amine from volatilizing out and entering and polluting an ion mobility spectrometry system. The validity and the easy analysis of the sample acquisition data are ensured, and the detection efficiency is greatly improved.
The chemical reagent can accept lone pair electrons of ammonia gas, so that ammonia gas and/or volatile organic amine in a substance to be detected are chemically fixed, the influence of ammonia gas and/or volatile organic amine signals can be effectively reduced, meanwhile, volatilization of other substances in a sample is not influenced, other substances are not damaged, and adverse effects on an instrument are not generated.
The invention provides a new thought aiming at sample ammonia and/or volatile organic amine signal inhibition, and the scientificity and effectiveness of the thought are verified through the trial of various reagents.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an ion transfer tube structure;
FIG. 2 is a flow chart of a biological sample detection;
FIG. 3 is a GC-IMS spectrum;
FIG. 4 is a graph showing the effect of other reactive ions on the spectrum;
FIG. 5 is a graph showing the results of ammonia and volatile organic amine signaling after continuous 3-needle sample injection of untreated urine;
FIG. 6 is a graph showing the results of ammonia and volatile organic amine signaling after continuous 6-needle sample injection of aspartic acid (Asp) added urine;
FIG. 7 is a graph showing the comparison of Asp treatment groups and ammonia gas and volatile organic amine signal spectra of different intensities;
FIG. 8 is a graph showing the results of ammonia and volatile organic amine signals after continuous 6-needle sample injection of blood with glutamic acid addition;
FIG. 9 is a graph showing the results of ammonia and volatile organic amine signals after continuous 6-needle injection of sulfuric acid-added tea leaves;
FIG. 10 is a graph showing the results of ammonia and volatile organic amine signaling after continuous 6-needle injection of aspartic acid (Asp) added shrimp meat;
FIG. 11 is a graph showing the results of ammonia and volatile organic amine signals after continuous 6-needle sample injection of fish meat with silver nitrate addition;
FIG. 12 is a graph showing the results of ammonia and volatile organic amine signaling after continuous sample introduction of proline treated urine;
FIG. 13 is a graph showing the results of ammonia and volatile organic amine signaling after continuous 3-needle sampling of untreated blood;
FIG. 14 is a graph showing the results of ammonia and volatile organic amine signaling after continuous 3-needle injection of untreated tea;
FIG. 15 is a graph showing the results of ammonia and volatile organic amine signals after continuous 3-needle sample injection of untreated shrimp meat;
FIG. 16 is a graph showing the results of ammonia and volatile organic amine signals after continuous 3-needle injection of untreated fish meat,
FIG. 17 is a graph showing the results of ammonia and volatile organic amine signaling after continuous sample introduction of mercuric chloride-treated urine;
FIG. 18 is a graph showing the results of volatile organic amine signaling after continuous sample injection of aspartic acid treated crab meat;
FIG. 19 is a graph showing the results of volatile organic amine signaling after continuous sample injection of untreated crab meat.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
In this embodiment, a urine sample is used as a sample to be tested, and the sample to be tested is treated with a chemical reagent.
The pipette draws 2mL of urine sample and injects the urine sample into a 20mL headspace bottle, 0.2g of aspartic acid is weighed and added, the mixture is slightly shaken and mixed, at the moment, the amino acid is excessive, solid precipitation of the amino acid can be observed at the bottom of the bottle, and the bottle cap is screwed to be measured. The temperature of the incubator is set to be 100 ℃, the incubation time is 5min, the headspace sample injection volume is 1000 mu L, and the single-needle analysis time is 15min.
The parameters of the ion mobility spectrum are as follows:
| Time (Time node) | EPC1 (drift gas flow) | EPC2 (Carrier gas flow) | Record (Record spectrogram) |
| 00:00,000 | 150mL/min | 2ml/min | Rec (begin acquisition record) |
| 02:00,000 | 150mL/min | 2ml/min | - |
| 20:00,000 | 150mL/min | 100ml/min | Stop (end of analysis of the sample) |
As shown in the results of the continuous 6-needle sample injection referring to FIG. 6, at the same position of the spectrogram, signals of ammonia and volatile organic amine do not appear, the signal intensity at the corresponding position is very low, and no trend of increasing accumulated signals exists.
Example 2
In this embodiment, a blood sample is used as a sample to be measured, and the sample to be measured is treated with a chemical reagent.
The pipette draws 500. Mu.L of blood sample into a 20mL headspace bottle, weighs and adds 0.1g of glutamic acid, and mixes with slight shaking, at which time the amino acid is excessive, solid precipitation of the amino acid can be observed at the bottom of the bottle, and the bottle cap is screwed up to be measured. The incubator temperature was set at 60 ℃, incubation time was 5min, headspace sample volume was 1000 μl, single needle analysis time was 15min.
Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As shown in the results of the continuous 6-needle sample injection referring to FIG. 8, at the same position of the spectrogram, signals of ammonia and volatile organic amine do not appear, the signal intensity at the corresponding position is very low, and no trend of increasing accumulated signals exists.
Example 3
In this embodiment, a tea sample is used as a sample to be tested, and the sample to be tested is treated with a chemical reagent.
1G of tea sample is weighed by a balance and transferred into a 20mL headspace bottle, 2mL of 0.01M1/2H 2SO4 is weighed and added, the mixture is slightly shaken and mixed, and a bottle cap is screwed for testing. The temperature of the incubator is set at 80 ℃, the incubation time is 10min, the headspace sample injection volume is 500 mu L, and the single-needle analysis time is 20min. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As shown in FIG. 9, the continuous 6-needle sample injection results show that at the same position of the spectrogram, signals of ammonia and volatile organic amine do not appear, the signal intensity at the corresponding position is very low, and no trend of increasing accumulated signals exists.
Example 4
In the embodiment, the shrimp meat is used as a sample to be tested, and the shrimp meat is treated with a chemical reagent.
2G of shrimp meat sample is weighed by a balance and transferred into a 20mL headspace bottle, 0.5g of aspartic acid is weighed and added, 2mL of water is added, the mixture is slightly shaken and mixed, and a bottle cap is screwed for testing. The incubator temperature was set at 60℃for 15min, the headspace sample volume was 500. Mu.L, and the single needle analysis time was 30min. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As shown in the results of the continuous 6-needle sample injection referring to FIG. 10, at the same position of the spectrogram, signals of ammonia gas and volatile organic amine do not appear, the signal intensity at the corresponding position is very low, and no tendency of increasing the accumulated signal exists.
Example 5
In this embodiment, fish meat is used as a sample to be tested, and the fish meat is treated with a chemical reagent.
2G of fish sample is weighed by a balance and transferred into a 20mL headspace bottle, 0.2g of silver nitrate is weighed and added, 2mL of water is added, the mixture is slightly shaken and mixed, and a bottle cap is screwed for testing. The incubator temperature was set at 60℃for 15min, the headspace sample volume was 500. Mu.L, and the single needle analysis time was 30min. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As shown in FIG. 11, the continuous 6-needle sample injection results show that the signals of ammonia and volatile organic amine do not appear at the same position of the spectrogram, the signal intensity at the corresponding position is very low, and the accumulated signal does not tend to increase.
Example 6
In this embodiment, a urine sample is used as a sample to be tested, and the sample to be tested is treated with a chemical reagent.
The pipette sucks 2mL of urine sample, injects the urine sample into a 20mL headspace bottle, weighs and adds 0.2g of mercuric chloride, slightly shakes and mixes, and screws up the bottle cap to be measured. The temperature of the incubator is set to be 100 ℃, the incubation time is 5min, the headspace sample injection volume is 1000 mu L, and the single-needle analysis time is 15min. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As shown in fig. 17, the continuous 6-needle sample injection results show that the signals of ammonia and volatile organic amine do not appear at the same position of the spectrogram, the signal intensity at the corresponding position is very low, and the accumulated signal does not tend to increase.
Example 7
In the embodiment, crabs are used as samples to be tested, and the samples are treated by chemical reagents.
1G of crab meat sample is weighed by a balance and transferred into a 20mL headspace bottle, 0.2g of aspartic acid is weighed and added, 2mL of water is added, the mixture is slightly shaken and mixed, and a bottle cap is screwed for testing. The incubator temperature was set at 60℃for 15min, the headspace sample volume was 500. Mu.L, and the single needle analysis time was 30min. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As shown in fig. 18, the continuous 6-needle sample injection results show that dimethylamine and trimethylamine signals do not appear at the same position of the spectrogram, the signal intensity at the corresponding position is very low, and no tendency exists for the accumulated signal to increase.
Comparative example 1
The comparative example uses a urine sample as the sample to be tested, and differs from example 1 in that no elimination of ammonia and volatile organic amine signals is performed. Directly and continuously injecting 3-needle samples. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As a result, referring to FIG. 5, after continuous sample injection of untreated urine, very strong signals of ammonia and volatile organic amine are observed on the left side of the RIP peak, as shown in the box of FIG. 5, and the signal intensity is gradually increased.
Comparative example 2
The difference compared to example 1 is that the elimination of ammonia and volatile organic amine signals is performed with neutral amino acids, the rest of the steps being identical. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As a result, referring to fig. 12, a smaller signal of ammonia and volatile organic amine was observed to the left of the RIP peak after continuous sample introduction of proline-treated urine, which was smaller than that of untreated urine, but the signal intensity still increased gradually.
Comparative example 3
The comparative example uses a blood sample as a sample to be tested, and is different from example 2 in that no elimination of ammonia and volatile organic amine signals is performed. Directly and continuously injecting 3-needle samples. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As a result, referring to FIG. 13, after continuous sample injection of untreated blood, very strong signals of ammonia gas and volatile organic amine are observed on the left side of the RIP peak, as shown in the box of FIG. 13, and the signal intensity is gradually increased.
Comparative example 4
In this comparative example, a tea leaf sample was used as a sample to be tested, and compared with example 3, the difference was that no elimination of ammonia gas and volatile organic amine signals was performed. Directly and continuously injecting 3-needle samples. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As a result, referring to FIG. 14, after continuous injection of untreated tea leaves, very strong signals of ammonia gas and volatile organic amine are observed on the left side of the RIP peak, as shown in the box of FIG. 14, and the signal intensity is gradually increased.
Comparative example 5
The comparative example uses a shrimp meat sample as the sample to be tested, and differs from example 4 in that no elimination of ammonia and volatile organic amine signals was performed. Directly and continuously injecting 3-needle samples. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As a result, referring to FIG. 15, after continuous sample injection of untreated shrimp meat, very strong signals of ammonia gas and volatile organic amine were observed on the left side of the RIP peak, as shown in the box of FIG. 15, and the signal intensity was gradually increased.
Comparative example 6
The comparative example uses a fish sample as a sample to be tested, and is different from example 5 in that no elimination of ammonia and volatile organic amine signals is performed. Directly and continuously injecting 3-needle samples. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As a result, referring to FIG. 16, after continuous sample injection of untreated fish meat, very strong signals of ammonia gas and volatile organic amine are observed on the left side of the RIP peak, as shown in the box of FIG. 16, and the signal intensity is gradually increased.
Comparative example 7
The comparative example uses a crab meat sample as the sample to be tested, and differs from example 7 in that no elimination of the volatile organic amine signal is performed. Directly and continuously injecting 3-needle samples. Other parameters of ion mobility spectrometry are the same as in example 1 except for this.
As a result, referring to FIG. 19, after continuous sample injection of untreated crab meat, very strong volatile organic amine signals (dimethylamine, trimethylamine) were observed to the left of the RIP peak, as shown in the box of FIG. 19, with increasing signal intensity.
Experimental example 1
The experimental example is used for researching the influence of signal detection of molecules to be detected after accumulating ammonia with different intensities.
As shown in fig. 7, the first spectrum on the left side is the Asp treatment group of example 1, the middle is the spectrum with weaker signals of ammonia and volatile organic amine, and the third is the spectrum with higher intensity after accumulation of ammonia and volatile organic amine. The signal Intensity graph is shown below in FIG. 7, and the signal intensities of ammonia and volatile organic amines can be quantified, see the Intensity column, which is the signal Intensity of ammonia and volatile organic amines in V volts. Ammonia and volatile organic amine are generally not known to be strong or weak before loading, and even if ammonia and volatile organic amine are weak, they accumulate to affect subsequent detection, so that inhibition is required as long as they exist. The different ammonia gas intensity sample data in this experimental example were derived from the first and last needles of the same ammonia gas containing sample. The peak position and intensity of the signal of the object to be detected between the two previous spectrograms are similar, and at the moment, the signals of ammonia and volatile organic amine are weaker, so that the peak signal of the molecule of the object to be detected is not influenced obviously. And compared with the third spectrogram, the signals of the ammonia and the volatile organic amine greatly influence the signals of the molecules of the object to be detected after the intensity of the ammonia is accumulated, and the peak position and the intensity are obviously changed.
Taken together, asp has a very remarkable effect on inhibiting volatilization and signal generation of ammonia and volatile organic amines, and preventing ammonia and volatile organic amines from entering and contaminating a GC-IMS system. Asp has no volatility, strong oxidability, no influence on other substances to form peaks and no damage to other volatile components, and is an effective method for inhibiting ammonia and/or volatile organic amine signals in biological sample detection.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
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| CN103675080A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院大连化学物理研究所 | Headspace sampler and ion mobility spectrometry combined system |
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| CN103675080A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院大连化学物理研究所 | Headspace sampler and ion mobility spectrometry combined system |
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