CN106018005A - Sampling pipe for detecting carbonyl compounds in electronic atomization steam of electronic cigarette as well as preparation method and application of sampling pipe - Google Patents
Sampling pipe for detecting carbonyl compounds in electronic atomization steam of electronic cigarette as well as preparation method and application of sampling pipe Download PDFInfo
- Publication number
- CN106018005A CN106018005A CN201610471617.0A CN201610471617A CN106018005A CN 106018005 A CN106018005 A CN 106018005A CN 201610471617 A CN201610471617 A CN 201610471617A CN 106018005 A CN106018005 A CN 106018005A
- Authority
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- China
- Prior art keywords
- sampling tube
- silica gel
- sampling
- gel particle
- electronic cigarette
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000005070 sampling Methods 0.000 title claims abstract description 215
- 150000001728 carbonyl compounds Chemical class 0.000 title claims abstract description 65
- 239000003571 electronic cigarette Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000889 atomisation Methods 0.000 title abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 137
- 239000000741 silica gel Substances 0.000 claims abstract description 133
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 133
- 239000002245 particle Substances 0.000 claims abstract description 113
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 35
- 238000001212 derivatisation Methods 0.000 claims abstract description 35
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 229920000742 Cotton Polymers 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 97
- 229910052757 nitrogen Inorganic materials 0.000 claims description 49
- 238000010521 absorption reaction Methods 0.000 claims description 24
- 238000010926 purge Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 19
- 239000007943 implant Substances 0.000 claims description 18
- 239000000779 smoke Substances 0.000 claims description 18
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 12
- 229920001971 elastomer Polymers 0.000 claims description 9
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 8
- 239000012047 saturated solution Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 230000006315 carbonylation Effects 0.000 claims description 6
- 238000005810 carbonylation reaction Methods 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 5
- 229920005479 Lucite® Polymers 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 2
- 238000010408 sweeping Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 238000004458 analytical method Methods 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 11
- 229960001866 silicon dioxide Drugs 0.000 abstract 3
- 238000005238 degreasing Methods 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 45
- HORQAOAYAYGIBM-UHFFFAOYSA-N 2,4-dinitrophenylhydrazine Chemical compound NNC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HORQAOAYAYGIBM-UHFFFAOYSA-N 0.000 description 20
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 13
- 230000000391 smoking effect Effects 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 150000001299 aldehydes Chemical class 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000010276 construction Methods 0.000 description 6
- -1 polyethylene terephthalate Polymers 0.000 description 6
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000010923 batch production Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 238000012387 aerosolization Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000001007 puffing effect Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 2
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000006199 nebulizer Substances 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 210000002345 respiratory system Anatomy 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
- KNMFWUYWAIBFIB-UHFFFAOYSA-N C(C)#N.[N+](=O)([O-])C1=C(C=CC(=C1)[N+](=O)[O-])NN Chemical compound C(C)#N.[N+](=O)([O-])C1=C(C=CC(=C1)[N+](=O)[O-])NN KNMFWUYWAIBFIB-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 230000001886 ciliary effect Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 description 1
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 description 1
- 238000005138 cryopreservation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 150000007857 hydrazones Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- ICIWUVCWSCSTAQ-UHFFFAOYSA-N iodic acid Chemical class OI(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-N 0.000 description 1
- 150000002496 iodine Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- LGROKZMEHJZWDU-UHFFFAOYSA-N n-amino-n-phenylnitramide Chemical compound [O-][N+](=O)N(N)C1=CC=CC=C1 LGROKZMEHJZWDU-UHFFFAOYSA-N 0.000 description 1
- 229960002715 nicotine Drugs 0.000 description 1
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0047—Organic compounds
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Combustion & Propulsion (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a sampling pipe for detecting carbonyl compounds in electronic atomization steam of an electronic cigarette as well as a preparation method and an application of the sampling pipe. The sampling pipe comprises a pipe body with two open ends, wherein the inside of the pipe body is filled with silica-gel particles, two ends of each silica-gel particle are blocked with degreasing cotton, and derivatization reagents capable of being subjected to a derivatization reaction with carbonyl compounds are adsorbed on surfaces of the silica-gel particles. The sampling pipe is simple in structure, relatively small in size and capable of preserving the carbonyl compounds for a long time and has great practical popularization and application value. The invention further provides a preparation method of the sampling pipe for detecting the carbonyl compounds in electronic atomization steam of the electronic cigarette, the method is simple and easy to operate and suitable for large-scale production of the sampling pipe. The invention further provides an application of the sampling pipe in quantitative detection of the carbonyl compounds in the atomization steam of the electronic cigarette, the sampling process and the follow-up analysis process are simple, the analysis time is relatively short, and the sampling pipe can detect the content of the carbonyl compounds in the atomization steam of the electronic cigarette accurately.
Description
Technical field
The present invention relates to electronic cigarette product physical and chemical inspection technical field, be specifically related to a kind of for detecting electronic cigarette atomizing steaming
Sampling tube of carbonyl compound and its preparation method and application in vapour.
Background technology
Electronic cigarette is a kind of through nebulizer, ree-oil to be converted into atomizing steam, and transmits nicotine and other things to respiratory system
The electronic installation of matter.Volatile carbonyl compound is an important harmful substance of class in electronic cigarette atomizing steam, abroad as far back as 20 generation
Record and the most carried out the research work of related fields the twenties, and this compounds is listed in 44 kinds of harmful components " Huffman is clear
Single ".Wherein low molecule carbonyl compound (referring mainly to formaldehyde, acetaldehyde and acrylic aldehyde) has ciliary toxicity, meeting in aspiration procedure
Stimulate respiratory system and the sensory organ of human body to some extent.
At present, more for the research of carbonyl compound in main flume both at home and abroad, main employing high performance liquid chromatography is divided
Analysis method.State Tobacco Monopoly Bureau of China issued YC/T 254-2008 industry standard in 2008, and the method uses through 2,4-bis-
Carbonyl compound in the glass fiber filter absorption flue gas that nitrophenyl hydrazine solution processed.International Tissues of Tobacco CORESTA sends out
The absorption plant of the 2,4 dinitrophenyl hydrazine acetonitrile solution after selecting in the CRM 74 of cloth equipped with quantitatively acidifying.But these methods are deposited
Loaded down with trivial details in processing procedure, analysis time, longer grade was not enough.
Summary of the invention
For solving the problems referred to above, the invention provides a kind of for detecting adopting of carbonyl compound in electronic cigarette atomizing steam
Sample pipe.This sampling tube simple in construction, it is possible to the accurately carbonyl compound content in detection electronic cigarette atomizing steam；The present invention also carries
The preparation method and application of this sampling tube are supplied.
First aspect present invention provides a kind of for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam, institute
Stating the body that sampling tube includes having two openings, described tubular body is filled with silica gel particle, the two of described silica gel particle
End blocks by loose implant, and described silica gel particle surface is adsorbed with can be with the derivatization of carbonyl compound generation derivative reaction
Reagent.
Wherein, described tubular body is filled with two sections of silica gel particles, by loose implant between described two sections of silica gel particles
Separate.
Wherein, described derivatization reagent is the 2,4 dinitrophenyl hydrazine of acidifying.
Wherein, the particle diameter of described silica gel particle is 20-40 mesh.
Wherein, at least one opening of described body is arranged to thin oral area, and one end of described thin oral area is filled with loose
Thing contacts, and other end rubber cap seals, and fills described silica gel particle at described thin oral area.
Wherein, the configuration of described thin oral area is hourglass ampuliform.
Wherein, the material of described body is lucite, quartz glass or transparent resin.
Wherein, described loose implant is absorbent cotton, organic cotton or glass fibre.
What first aspect present invention provided is used for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam, adsorbs and exists
Derivatization reagent on silica gel particle and the carbonyl compound generation derivative reaction in electronic cigarette atomizing steam, generate hydrazone class
Compound, is used directly for subsequent quantitation detection and analyzes, simple to operate, and can accurately detect electronic cigarette electronic cigarette atomizing steam
In carbonyl compound content.Additionally, the silica gel particle in sampling tube is cheap and easy to get, cost is relatively low, silica gel particle specific surface area
Greatly, it is easy to absorption, it is easy to eluting；The sampling tube simple in construction that the present invention provides, small volume, holding time are long, are suitable for batch
Produce, there is the highest practical extending application value.
Second aspect present invention provides a kind of for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam
Preparation method, comprises the following steps:
(1) take a body with two openings, silica gel particle is filled in the inside of described body, then by described
The two ends of silica gel particle block by loose implant；
(2) in described body, add derivatization reagent, make derivatization reagent described in the surface adsorption of described silica gel particle；
(3) body described in dried remove the liquid in body, obtains for detecting carbonyl in electronic cigarette atomizing steam
The sampling tube of based compound.
Wherein, before described step (1), further comprise the steps of: at least one opening to described body and carry out at heating
Reason, and described opening is drawn high in thin oral area.
Wherein, before adding described derivatization reagent in described body, in described body, first add eluting solvent, go
Impurity except described silica gel particle surface.
Wherein, the operation of the liquid in described dry removal body is: use nitrogen purging device in described sampling tube
Being passed through nitrogen, to dry up the liquid removed in body, described nitrogen purging device includes the nitrogen source being sequentially connected with, equipped with saturated iodine
Change the first GAS ABSORPTION bottle of potassium solution and equipped with the second GAS ABSORPTION bottle of derivatization reagent.
What second aspect present invention provided is used for detecting the preparation of the sampling tube of carbonyl compound in electronic cigarette atomizing steam
Method, method is simple to operation, and the sampling tube prepared is used directly for carbonyl compound in Subsequent electronic aerosolization steam
Quantitative detecting analysis, meanwhile, sampling tube simple in construction, easy to make, volume is little, the holding time is long, it is suitable for batch production.
Third aspect present invention provides a kind of sampling tube as described in relation to the first aspect and steams at detection by quantitative electronic cigarette atomizing
The application of carbonyl compound in vapour, comprises the following steps:
The suction nozzle of one end of sampling tube with electronic smoke atomizer is tightly connected, the atomization that described electronic smoke atomizer is discharged
Steam is entered in described sampling tube by described suction nozzle again, and is discharged by the other end in described sampling tube, now, and described atomization
Carbonyl compound in steam is with the derivatization reagent generation derivative reaction in described sampling tube thus is captured；
After sampling terminates, take out the silica gel particle in described sampling tube, in described silica gel particle, then add desorbing molten
Agent, after subsequently the solvent after desorbing being centrifuged 5-10min, uses high performance liquid chromatograph-UV-detector to carry out by supernatant
Detection, obtains the content of carbonyl compound in described electronic cigarette atomizing steam.
Third aspect present invention provides described sampling tube carbonyl compound in detection by quantitative electronic cigarette atomizing steam
Application, the method may be used for the quantitative detecting analysis of carbonyl compound in electronic cigarette atomizing steam, sampling process and follow-up point
Analysis process is simple, and analysis time is shorter, can accurately detect the carbonyl compound content in electronic cigarette atomizing steam simultaneously.
To sum up, beneficial effect of the present invention includes the following aspects:
1, the sampling tube simple in construction that the present invention provides, small volume, holding time are long, and having the highest actual popularization should
By value；
What 2, the present invention provided is used for detecting the preparation method of the sampling tube of carbonyl compound in electronic cigarette atomizing steam, side
Method is simple to operation, is suitable for batch production, and the sampling tube prepared is used directly for carbonylation in Subsequent electronic aerosolization steam
The quantitative detecting analysis of compound；
3, the sampling tube that the present invention provides can apply to carbonyl compound in detection by quantitative electronic cigarette atomizing steam, sampling
Process and subsequent analysis process are simple, and analysis time is shorter, can accurately detect in electronic cigarette electronic cigarette atomizing steam simultaneously
Carbonyl compound content.
Accompanying drawing explanation
The sampling tube schematic diagram that Fig. 1 provides for the embodiment of the present invention 1；
The sampling tube schematic diagram that Fig. 2 provides for the embodiment of the present invention 2；
The nitrogen purging device schematic diagram that Fig. 3 provides for the embodiment of the present invention 3；
The sampling tube that Fig. 4 provides for the embodiment of the present invention 5 sampling efficiency figure in the case of difference suction quantity；
The sampling tube that Fig. 5 provides for the embodiment of the present invention 5 formaldehyde sampling efficiency figure under the different holding times；
The sampling tube that Fig. 6 provides for the embodiment of the present invention 5 acetaldehyde sampling efficiency figure under the different holding times；
The sampling tube that Fig. 7 provides for the embodiment of the present invention 5 acrylic aldehyde sampling efficiency figure under the different holding times；
Fig. 8 is the chromatogram of the embodiment of the present invention 6 empty solution；
Fig. 9 is the chromatogram of the carbonyl complex in the sample that in the embodiment of the present invention 6, first sampling tube collects；
Figure 10 is the chromatograph of the carbonyl complex in the sample that in the embodiment of the present invention 6, second sampling tube collects
Figure.
Detailed description of the invention
The following stated is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as
Protection scope of the present invention.
First aspect present invention provides a kind of for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam, adopts
Sample pipe includes the body with two openings, and tubular body is filled with silica gel particle, and the two ends of silica gel particle are filled with loose
Thing blocks, and silica gel particle surface is adsorbed with can be with the derivatization reagent of carbonyl compound generation derivative reaction.
The body that the present invention provides has two openings, it is simple to filling or take out silica gel particle wherein, body is permissible
Reuse.
In an embodiment of the present invention, the material of body is lucite, quartz glass or transparent resin.
In the present invention one preferred implementation, transparent resin can be polymethyl methacrylate (PMMA), Merlon
(PC), polystyrene (PS), polyethylene terephthalate (PET) or ethylene glycol terephthalate-1,4-hexamethylene two
Methanol ester (PETG).
In an embodiment of the present invention, carbonyl compound is formaldehyde, acetaldehyde, acetone, acrylic aldehyde, propionic aldehyde, crotonic aldehyde, 2-fourth
One or more in ketone and butyraldehyde.
In an embodiment of the present invention, the internal diameter of body does not limits, such as, may be selected to be 4-10mm.
In an embodiment of the present invention, the length of body does not limits, such as, may be selected to be 5-20cm.
In an embodiment of the present invention, body two ends rubber cap seals.The impurity in environment so can be avoided to enter
Sampling tube affects the performance of silica gel.
In an embodiment of the present invention, at least one opening of body is arranged to thin oral area, and one end of thin oral area is with thin
Pine implant contact, other end rubber cap seals, and at thin oral area filling gel granule.
Being provided with thin oral area in sampling tube body of the present invention, subsequent sampling pipe is for gathering the carbonyl in electronic cigarette atomizing steam
During compound, thin oral area can avoid the loose implant in sampling tube to be entrained by the flow of air.
In an embodiment of the present invention, the concrete diameter of thin oral area is not done particular determination, as long as not affecting sampling
The preparation of pipe and electronic cigarette atomizing steam are collected.
In an embodiment of the present invention, the configuration of thin oral area is hourglass ampuliform.
In an embodiment of the present invention, silica gel particle is solid absorption silica gel particle.
In an embodiment of the present invention, silica gel particle is column layer chromatography silicone rubber granule.
In an embodiment of the present invention, the particle diameter of silica gel particle is 20-40 mesh.
In an embodiment of the present invention, in sampling tube, the weight of silica gel particle does not limits, such as, can be 100-600mg.
In an embodiment of the present invention, the two ends of silica gel particle are with loose implant closure, to fix silica gel particle.
In the present invention one preferred implementation, loose implant is absorbent cotton, organic cotton or glass fibre.
In an embodiment of the present invention, tubular body can fill one section of silica gel particle can also fill multistage silica gel
Grain.
In an embodiment of the present invention, tubular body is filled with two sections of silica gel particles, with loose between two sections of silica gel particles
Implant separates.
In the present invention one preferred implementation, body includes the first opening and the second opening being oppositely arranged, two sections
Silica gel particle is respectively first paragraph silica gel particle and second segment silica gel particle, first paragraph silica gel particle near the first opening,
Two-stage nitration silica gel particle separates by loose implant near between the second opening, two sections of silica gel particles, second segment silica gel particle
Weight is more than the weight of first paragraph silica gel particle.
In an embodiment of the present invention, the weight of first paragraph silica gel particle is 20-100mg, the weight of second segment silica gel particle
Amount is 200-300mg.
The present invention fills two sections of silica gel particles at tubular body, and the silica gel particle near the first opening can be as buffering
District, it is to avoid in sampling tube preparation process, in air and high pure nitrogen, aldehyde material reacts with 2,4 dinitrophenyl hydrazine, causes sample
Pipe mass uniformity is poor, affects subsequent sample measurement result.The silica gel of first paragraph, before sample collecting, is poured out by this sampling tube
, follow-up employing second segment silica gel particle traps the carbonyl compound in electronic cigarette atomizing steam.
In an embodiment of the present invention, derivatization reagent is the 2,4 dinitrophenyl hydrazine of acidifying.
In an embodiment of the present invention, derivatization reagent is the 2,4 dinitrophenyl hydrazine of phosphoric acid.
In an embodiment of the present invention, for detect the sampling tube of carbonyl compound in electronic cigarette atomizing steam be stored in-
Under the conditions of 20 to-4 DEG C.
What first aspect present invention provided is used for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam, this sampling
Pipe has the advantage that the derivatization reagent and carbonyl in electronic cigarette atomizing steam adsorbing on silica gel particle in (1) sampling tube
Compound generation derivative reaction, generates hydrazone compounds, and this sampling tube is used directly for subsequent quantitation detection and analyzes, operation
Simply, and can accurately detect the carbonyl compound content in electronic cigarette atomizing steam；(2) silica gel particle is cheap and easy to get, cost
Relatively low, meanwhile, silica gel particle specific surface area is big, it is easy to absorption, it is easy to eluting；(3) sampling tube simple in construction, easy to make, body
Long-pending little, the holding time is long, be suitable for batch production, there is the highest practical extending application value.
Second aspect present invention provides a kind of for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam
Preparation method, comprises the following steps:
(1) take a body with two openings, silica gel particle is filled in the inside of body, then by silica gel particle
Two ends with loose implant closure；
(2) in body, add derivatization reagent, make the surface adsorption derivatization reagent of silica gel particle；
(3) dried body remove the liquid in body, obtains for detecting carbonylation in electronic cigarette atomizing steam
The sampling tube of compound.
In an embodiment of the present invention, the material of body is lucite, quartz glass or transparent resin.
In the present invention one preferred implementation, transparent resin can be polymethyl methacrylate (PMMA), Merlon
(PC), polystyrene (PS), polyethylene terephthalate (PET) or ethylene glycol terephthalate-1,4-hexamethylene two
Methanol ester (PETG).
In an embodiment of the present invention, before step (1), further comprise the steps of: after body ultrasonic cleaning, use deionized water
Rinse, dry at 105 DEG C.
In an embodiment of the present invention, before step (1), further comprise the steps of: at least one opening to body and carry out
Heat treated, and opening is drawn high in thin oral area.
In the present invention one preferred implementation, heat in the position of distance opening end about 0.5cm, press from both sides with tweezers
Thin oral area is formed after holding.
In an embodiment of the present invention, the configuration of thin oral area is hourglass ampuliform.
In the present invention one preferred implementation, body includes the first opening and the second opening being oppositely arranged, two sections
Silica gel particle is respectively first paragraph silica gel particle and second segment silica gel particle, first paragraph silica gel particle near the first opening,
Two-stage nitration silica gel particle separates by loose implant near between the second opening, two sections of silica gel particles, second segment silica gel particle
Weight is more than the weight of first paragraph silica gel particle.
In an embodiment of the present invention, the weight of first paragraph silica gel is 20-100mg, and the weight of second segment silica gel is 200-
300mg。
The present invention fills two sections of silica gel particles at tubular body, near the silica gel particle of the first opening as relief area,
Avoid in sampling tube preparation process aldehyde material in air and high pure nitrogen to react with 2,4 dinitrophenyl hydrazine, cause sample cell matter
Amount homogeneity is poor, affects subsequent sample measurement result.The silica gel particle of first paragraph, before sample collecting, is poured out by this sampling tube
, follow-up employing second segment silica gel particle traps the carbonyl compound in electronic cigarette atomizing steam.
In an embodiment of the present invention, before adding derivatization reagent in body, in body, first add eluting solvent,
Remove the impurity of silica gel particle surface.
In an embodiment of the present invention, eluting solvent is acetonitrile.
In an embodiment of the present invention, use syringe to inject 10ml acetonitrile to sampling tube, allow acetonitrile naturally drip, repeat
Operate twice.The purpose adding acetonitrile is to remove the impurity of silica gel particle surface.
In an embodiment of the present invention, derivatization reagent is the 2,4 dinitrophenyl hydrazine of acidifying.
In an embodiment of the present invention, the preparation method of derivatization reagent is: measure 2,4 dinitrophenyl hydrazine saturated solution
30mL is placed in 1000mL volumetric flask, is subsequently adding 500mL acetonitrile, adds 1mL phosphoric acid, shakes up, and obtains the 2 of acidifying, 4-bis-
Nitrophenyl hydrazine.
In an embodiment of the present invention, the derivatization reagent using syringe to add 10-20mL in sampling tube, allow derivative
Change reagent naturally to drip.The amount of derivatization reagent is excessive for the amount of silica gel particle.
In an embodiment of the present invention, being passed through nitrogen to sampling tube, purging removes the liquid in body.
In an embodiment of the present invention, the flow velocity of nitrogen is 400ml/min, and purge time is 5-10min.
In an embodiment of the present invention, the operation being dried the liquid removed in body is: use nitrogen purging device to adopting
Being passed through nitrogen in sample pipe, to dry up the liquid removed in body, nitrogen purging device includes the nitrogen source being sequentially connected with, equipped with saturated
First GAS ABSORPTION bottle of liquor kalii iodide and the second GAS ABSORPTION bottle equipped with derivatization reagent.
When nitrogen in nitrogen source passes through the first GAS ABSORPTION bottle equipped with saturated solution of potassium iodide, saturated solution of potassium iodide can
To absorb the ozone in nitrogen, it is to avoid ozone reacts with the derivatization reagent in sampling tube thus subsequent sampling result is produced shadow
Ring.Nitrogen is by during equipped with the second GAS ABSORPTION bottle of derivatization reagent, in nitrogen in aldehyde material and the second GAS ABSORPTION bottle
2,4 dinitrophenyl hydrazine generation derivative reaction, thus remove aldehyde material in nitrogen, it is to avoid in nitrogen, aldehyde material is to rear
Continuous sampling interferes.
In an embodiment of the present invention, when sampling tube arranges two sections of silica gel particles, it is passed through nitrogen, nitrogen to sampling tube
Entered in first paragraph silica gel particle by the first opening, first paragraph silica gel particle can with nitrogen aldehyde material that may be present
React to remove impurity that may be present in nitrogen Deng impurity, then enter back in second segment silica gel particle.Prepare adopts
First paragraph silica gel particle in sampling tube before sampling, is first poured out, then by the suction nozzle of sampling tube Yu electronic smoke atomizer by sample pipe
It is connected, uses the carbonyl compound in second segment silica gel trapping electronic cigarette atomizing steam.
In an embodiment of the present invention, when nitrogen is dried the liquid removed in body, acetonitrile is used to clean tube wall
And end.The purpose that acetonitrile cleans is to rinse out and remains in pipe outer wall and the 2,4 dinitrophenyl hydrazine of sampling tube end, it is to avoid
Sampling process causes deviation.
In an embodiment of the present invention, obtain for detecting in electronic cigarette atomizing steam after the sampling tube of carbonyl compound,
Preserve under the conditions of this sampling tube is placed in-20 DEG C to-4 DEG C.
What second aspect present invention provided is used for detecting the preparation of the sampling tube of carbonyl compound in electronic cigarette atomizing steam
Method, method is simple to operation, and the sampling tube prepared is used directly for carbonyl compound in Subsequent electronic aerosolization steam
Quantitative detecting analysis, meanwhile, sampling tube simple in construction, easy to make, volume is little, the holding time is long, it is suitable for batch production.
Third aspect present invention provides the sampling tube of above-mentioned first aspect carbonyl in detection by quantitative electronic cigarette atomizing steam
The application of based compound, comprises the following steps:
The suction nozzle of one end of sampling tube with electronic smoke atomizer is tightly connected, the atomizing steam that electronic smoke atomizer is discharged
Entered in sampling tube by suction nozzle again, and discharged by the other end in sampling tube, now, the carbonylation in electronic cigarette atomizing steam
Compound is with the derivatization reagent generation derivative reaction in sampling tube thus is captured；
After sampling terminates, take out the silica gel particle in sampling tube, in silica gel particle, then add desorption solvent, the most right
After solvent after desorbing is centrifuged 5-10min, supernatant uses high performance liquid chromatograph-UV-detector detect, obtains
The content of the carbonyl compound in electronic cigarette atomizing steam.
In an embodiment of the present invention, when sampling tube is applied to carbonyl compound in detection by quantitative electronic cigarette atomizing steam,
At least two sampling tubes can be cascaded for sampling.
The suction nozzle of one end of sampling tube with electronic smoke atomizer is tightly connected by the present invention, and the other end is connected with smoking apparatus,
By the suction of smoking apparatus, the atomizing steam that electronic smoke atomizer is discharged is entered in sampling tube by suction nozzle, and by sampling tube
The other end discharge.
The structure of smoking apparatus is not done particular determination by the present invention, it is possible to passed through by the atomizing steam that electronic smoke atomizer is discharged
The device that suction nozzle enters in sampling tube can.
In an embodiment of the present invention, before sampling, the suction frequencies of smoking apparatus, suction time, suction number are first set
The smoking parameters such as amount, it is to avoid sampling tube sampling overload.
In an embodiment of the present invention, the method to set up of smoking parameters is: by three sampling tubes and the smoking apparatus phase of series connection
Even, setting the parameters such as suction frequencies, suction time, suction quantity, sample, suction measures each sampling respectively after terminating
The content of carbonyl compound in pipe, should detect carbonyl compound in the 3rd sampling tube, when the suction frequencies of correspondence, suction
Between, the suction parameter such as quantity may be used for subsequent sampling process.
The present invention is connected in series three sampling tubes for verifying sampling smoking parameters, only when not detecting in the 3rd sampling tube
During carbonyl complex, when could illustrate to select this puffing regimens, connect two sampling tubes and can detect electronic smoke completely
Change the compound to be checked in steam.When the 3rd sampling tube remains to detect carbonyl complex, then illustrate under this puffing regimens
Only can not collect the test substance in electronic cigarette atomizing steam completely with two sampling tubes, it is impossible to meet sampling request, in addition it is also necessary to
Adjust puff number, or increase the quantity of sampling tube.
In an embodiment of the present invention, the number of times of suction is 20 mouthfuls, and the time of suction is 3.0 seconds every time, and puff interval is
30 seconds, the electronic cigarette atomizing vapour volume of suction was 55mL every time.
In an embodiment of the present invention, body includes the first opening and the second opening being oppositely arranged, by a part
Silica gel particle is filled in the tubular body near the second opening, forms second segment silica gel, and the two ends of second segment silica gel are with loose
Implant blocks, and then continues to fill up silica gel particle in the position near the first opening, forms first paragraph silica gel, by first paragraph
The end of silica gel seals by loose implant, and the weight of second segment silica gel is more than the weight of first paragraph silica gel.
In an embodiment of the present invention, when sampling tube is provided with two sections of silica gel particles, before sampling by sampling tube
First paragraph silica gel particle pour out, then the suction nozzle of the first opening of sampling tube with electronic smoke atomizer is tightly connected and carries out
Sampling.
In an embodiment of the present invention, desorption solvent is acetonitrile.
In an embodiment of the present invention, in silica gel particle, add 5ml acetonitrile as desorption solvent.
Third aspect present invention provides a kind of sampling tube carbonyl compound in detection by quantitative electronic cigarette atomizing steam
Application, gathers carbonyl compound in electronic cigarette atomizing steam, sampling process and subsequent analysis process by sampling tube simple, analyzes
Time is shorter, can accurately detect the carbonyl compound content in electronic cigarette atomizing steam simultaneously.
Embodiment 1:
A kind of for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam, including having the first opening and
The body of two openings, the second opening of body is arranged to thin oral area, and tubular body is filled with silica gel particle, silica gel particle
Two ends with absorbent cotton block, silica gel particle surface be adsorbed with can with the derivatization reagent of carbonyl compound generation derivative reaction,
First opening and the second opening rubber cap seal.
The sampling tube schematic diagram that Fig. 1 provides for the embodiment of the present invention 1；As it is shown in figure 1,1 represent body in Fig. 1,11 represent
First opening of body, 12 represent the second opening of body, and 2 represent silica gel particle, and 3 represent absorbent cotton, and 4 represent thin mouth
Portion, 5 represent rubber cap.
Embodiment 2:
A kind of for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam, including having the first opening and
The body of two openings, the second opening of body is arranged to thin oral area, and tubular body is filled with two sections of silica gel particles, is respectively
First paragraph silica gel particle and second segment silica gel particle, the first end silica gel particle leans near the first opening, the second end silica gel particle
Nearly thin oral area, separates with absorbent cotton between two sections of silica gel particles, and the two ends of every section of silica gel particle absorbent cotton blocks, first paragraph
The weight of silica gel particle is 50mg, and the weight of second segment silica gel particle is 300mg, and silica gel particle surface is adsorbed with can be with carbonylation
The derivatization reagent of compound generation derivative reaction, the first opening and the second opening rubber cap seal.
The sampling tube schematic diagram that Fig. 2 provides for the embodiment of the present invention 2；As in figure 2 it is shown, 1 represent body in Fig. 2,11 represent
First opening of body, 12 represent the second opening of body, and 21 represent first paragraph silica gel particle, and 22 represent second segment silica gel
Granule, 3 represent absorbent cotton, and 4 represent thin oral area, and 5 represent rubber cap.
Embodiment 3:
A kind of for detecting the preparation method of the sampling tube of carbonyl compound in electronic cigarette atomizing steam, including following step
Rapid:
(1) glass tubing (length * internal diameter * external diameter is 10cm*4mm*6mm) is taken, after ultrasonic cleaning, with deionized water rinsing,
Drying at 105 DEG C, glass tubing includes the first opening and the second opening being oppositely arranged, then with alcohol blast burner heating away from
Second opening port about 0.5cm position, tweezers clamping processes and is here formed as thin oral area.Weigh 20-40 mesh column layer chromatography silicone rubber
300mg (purchased from Shanghai Yi Ka Bioisystech Co., Ltd), is filled in glass tubing and forms first paragraph silica gel at thin oral area, and two
End absorbent cotton seals；Then filling 50mg silica gel formation second segment silica gel near the first open end, silica gel end is with de-
Fat minuteness seals；
(2) by standby for the saturated solution that is configured to 2,4 dinitrophenyl hydrazine after 2,4 dinitrophenyl hydrazine recrystallized from acetonitrile three times
With, measure 2,4 dinitrophenyl hydrazine saturated solution 30ml and put in 1000ml volumetric flask, add 500ml acetonitrile, accurate addition 1ml phosphorus
Acid, shakes up, and obtains 2,4 dinitrophenyl hydrazine solution.Take the body that step (1) obtains, the first end be connected with 10ml syringe,
Add 10ml acetonitrile, allow liquid naturally drip, repetitive operation twice.2,4 dinitrophenyl hydrazine is added when acetonitrile stops drippage
Solution 14.0ml, allows liquid naturally drip, and during to liquid stopping drippage, is connected with nitrogen purging device by body, and nitrogen purges
Device include the nitrogen source being sequentially connected with, the first GAS ABSORPTION bottle equipped with saturated solution of potassium iodide and equipped with derivatization reagent
Two GAS ABSORPTION bottles.Control nitrogen flow rate 400ml/min, persistently purge silica gel tube, and clean pipe outer wall and end with acetonitrile, blow
Take off body after sweeping about 5 minutes, body two ends rubber cap is sealed, obtains for detecting carbonylation in electronic cigarette atomizing steam
The sampling tube of compound, and in-20 DEG C of preservations.
The nitrogen purging device that Fig. 3 provides for the embodiment of the present invention 3；As it is shown on figure 3, nitrogen purging device includes connecting successively
The nitrogen source (not shown) that connects, equipped with the first GAS ABSORPTION bottle (b) of saturated solution of potassium iodide (d) with equipped with derivatization reagent
C second GAS ABSORPTION bottle (a) of (), in figure, arrow represents the flow direction of nitrogen.Sequentially pass through the first GAS ABSORPTION bottle and the second gas
The nitrogen of body absorption bottle enters and uses in pipe for being dried the liquid removed in sampling tube.
Embodiment 4:
A kind of sampling tube is the application of carbonyl compound in detection by quantitative electronic cigarette atomizing steam, comprises the following steps:
(1) sampling parameter is determined: be tightly connected with the suction nozzle of electronic smoke atomizer one end of three sampling tubes of series connection,
Setting the parameters such as suction frequencies, suction time, suction quantity, sample, the atomizing steam that electronic smoke atomizer is discharged is again
Being entered in sampling tube by suction nozzle, and discharged by the other end in sampling tube, sampling measures in each sampling tube after terminating respectively
The content of carbonyl compound, should detect carbonyl compound in the 3rd sampling tube.
(2) two sampling tube one end of series connection are tightly connected with the suction nozzle of electronic smoke atomizer, use in step (1) and set
The parameters such as fixed suction frequencies, suction time, suction quantity, sample.The atomizing steam that electronic smoke atomizer is discharged leads to again
Cross suction nozzle to enter in sampling tube, and discharged by the other end in sampling tube.After sampling terminates, take out the silica gel in sampling tube
Grain, then accurate addition 5ml acetonitrile in silica gel particle, is centrifuged the solvent after desorbing subsequently, after centrifugal 10 minutes, will
Supernatant uses high performance liquid chromatograph-UV-detector (HPLC-UV, 5 rich high performance liquid chromatograph LC100) detection, calculates
The content of the carbonyl compound in electronic cigarette atomizing steam.
Embodiment 5:
In order to determine optimal preparation parameter, sampling condition and the retention of sampling tube.Respectively to nitrogen purging device, nitrogen
Air-blowing flyback time, sampling smoking parameters and sampling tube preservation condition make following research experiment:
(1) effect of the second GAS ABSORPTION bottle a in nitrogen purging device is investigated: when only loading appropriate saturated iodate with one
When GAS ABSORPTION bottle (b) of potassium solution is as nitrogen purging device.Sampling tube manage in nitrogen purge in absorbent cotton and portion
Divide silica gel particle to be become red from yellow, may be that in nitrogen, aldehyde material and 2,4 dinitrophenyl hydrazine in sampling tube occur derivative
Change reaction.When increasing GAS ABSORPTION bottle (a) of another 2,4 dinitrophenyl hydrazine solution loading acidifying, with identical nitrogen
Purging condition prepares sampling tube, the situation of silica gel particle variable color does not occurs.Illustrate that the present invention arranges the second GAS ABSORPTION bottle permissible
Remove the aldehyde material in nitrogen, it is to avoid the aldehyde material in nitrogen and 2 on the silica gel particle in sampling tube, 4-dinitro benzene
Hydrazine reacts.
(2) the nitrogen purge time impact on the preparation of sampling tube: control nitrogen flow rate is 400ml/min, purges respectively
Sampling tube 3,5,10 minutes.When 3 minutes, in sampling tube, 2,4 dinitrophenyl hydrazine solution purges dry the most completely；When 5 minutes, sampling
Pipe solution removes substantially；Part silicone gel desorption 2,4 dinitrophenyl hydrazine in sampling tube when 10 minutes, silica gel is become white from yellow,
And import department's absorbent cotton is become red from yellow.
(3) smoking parameters sets: be tightly connected with the suction nozzle of electronic smoke atomizer one end of two sampling tubes of series connection,
The other end is connected to smoking apparatus, and the atomizing steam that electronic smoke atomizer is discharged is entered in sampling tube by suction nozzle again, and by sampling
The other end in pipe is discharged, fixing suction frequencies be aspirated once every 30 seconds, each suction time 3.0 seconds, each suction body
Long-pending 55ml, is respectively adopted 150 mouthfuls, 50 mouthfuls, 20 mouthfuls and same sample is carried out carbonyl complex detection.Testing result such as Fig. 4 institute
Show, the sampling tube that Fig. 4 provides for an embodiment of the present invention sampling efficiency figure in the case of difference suction quantity；From Fig. 4
It can be seen that along with puff count increases, aldehyde material concentration to be detected increases, and has part aldehyde material to penetrate sampling tube, adopts
Sample efficiency declines, and when aspirating 20 mouthfuls, sampling efficiency is 100%.
(4) the sampling tube preservation condition impact on using efficiency: prepare sampling tube, sampling tube is divided into 3 groups, preserves respectively
At 25 DEG C, 4 DEG C, at-20 DEG C, after 3,7,14,20 days, then take out sampling tube, measure same electricity with identical puffing regimens
Sub-cigarette sample, after eluting silica gel, HPLC analyzes, and does blank correction simultaneously.As shown in Figure 5-Figure 7, Fig. 5 is this to testing result
The sampling tube that bright embodiment 5 provides formaldehyde sampling efficiency figure under the different holding times；Fig. 6 provides for the embodiment of the present invention 5
Sampling tube acetaldehyde sampling efficiency figure under the different holding times；The sampling tube that Fig. 7 provides for the embodiment of the present invention 5 is in difference
Acrylic aldehyde sampling efficiency figure under holding time.From such as Fig. 5-Fig. 7 it can be seen that sampling tube at 4 DEG C in 14 days sampling effect
Rate is still more than 90%, it is known that sampling tube sampling efficiency when cryopreservation that the embodiment of the present invention provides is higher.
Embodiment 6
The mensuration of sampling tube useful load: (being called the first sampling tube and the second sampling tube, first adopts by two sampling tubes
In sample pipe and the second sampling tube, the weight of silica gel is essentially identical) it is cascaded, by one end of the first sampling tube and electronic cigarette (type
Number TRUVAPE Air, ree-oil taste is A, and in ree-oil, PG/VG ratio is 70%/30%) suction nozzle of nebulizer is tightly connected, and
One end of two sampling tubes is connected to smoking apparatus, fixing suction frequencies be aspirated once every 30 seconds, each suction time 3.0 seconds,
Draw volume 55ml, suction 150 mouthfuls every time, carries out HPLC and analyzes detection the carbonyl complex in sample.Two sampling tubes
Middle 2,4 dinitrophenyl hydrazine reacts the most completely.Sampling tube useful load is shown in Table 1, the chromatogram of the carbonyl complex in sample such as figure
Shown in 8-10 (in Fig. 8-10,1 represents DNPH peak, and 2 represent formaldehyde peak, and 3 represent acetaldehyde peak, and 4 represent acrylic aldehyde peak), Fig. 8 is blank
The chromatogram of solution, Fig. 9 is the chromatogram of the carbonyl complex in the sample that the first sampling tube collects, and Figure 10 is second
The chromatogram of the carbonyl complex in the sample that sampling tube collects.
Table 1 sampling tube useful load
--represent and do not detect.
It can be seen that the sampling tube that the present invention provides may be used for detecting electronic cigarette atomizing steam from table 1 and Fig. 8-10
In carbonyl compound.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (13)
1. one kind is used for detecting the sampling tube of carbonyl compound in electronic cigarette atomizing steam, it is characterised in that described sampling tube bag
Including the body with two openings, described tubular body is filled with silica gel particle, and the two ends of described silica gel particle are filled out with loose
Filling thing closure, described silica gel particle surface is adsorbed with can be with the derivatization reagent of carbonyl compound generation derivative reaction.
2. sampling tube as claimed in claim 1, it is characterised in that described tubular body is filled with two sections of silica gel particles, described
Separate by loose implant between two sections of silica gel particles.
3. sampling tube as claimed in claim 1, it is characterised in that described derivatization reagent is the 2 of acidifying, 4-dinitro benzene
Hydrazine.
4. sampling tube as claimed in claim 1, it is characterised in that the particle diameter of described silica gel particle is 20-40 mesh.
5. sampling tube as claimed in claim 1, it is characterised in that at least one opening of described body is arranged to thin mouth
Portion, one end of described thin oral area contacts with loose implant, and other end rubber cap seals, and fills described at described thin oral area
Silica gel particle.
6. sampling tube as claimed in claim 5, it is characterised in that the configuration of described thin oral area is hourglass ampuliform.
7. the sampling tube as described in claim 1 to 6 is arbitrary, it is characterised in that the material of described body is lucite, quartz
Glass or transparent resin.
8. sampling tube as claimed in claim 7, it is characterised in that described loose implant is absorbent cotton, organic cotton or glass
Fiber.
9. the preparation method of a sampling tube as claimed in claim 1, it is characterised in that comprise the following steps:
(1) take a body with two openings, silica gel particle is filled in the inside of described body, then by described silica gel
The two ends of granule block by loose implant；
(2) in described body, add derivatization reagent, make derivatization reagent described in the surface adsorption of described silica gel particle；
(3) body described in dried remove the liquid in body, obtains for detecting carbonylation in electronic cigarette atomizing steam
The sampling tube of compound.
10. the preparation method of sampling tube as claimed in claim 9, it is characterised in that before described step (1), also include step
Rapid: at least one opening of described body to be carried out heat treated, and described opening is drawn high in thin oral area.
The preparation method of 11. sampling tubes as claimed in claim 9, it is characterised in that add described derivative in described body
Before changing reagent, in described body, first add eluting solvent, remove the impurity of described silica gel particle surface.
The preparation method of 12. sampling tubes as claimed in claim 9, it is characterised in that the liquid in described dry removal body
Operation be: use nitrogen purging device to be passed through nitrogen in described sampling tube, to dry up the liquid removed in body, described nitrogen
Air-blowing sweeping device includes the nitrogen source being sequentially connected with, equipped with the first GAS ABSORPTION bottle of saturated solution of potassium iodide and tries equipped with derivatization
Second GAS ABSORPTION bottle of agent.
13. as described in any one of claim 1-8 sampling tube in detection by quantitative electronic cigarette atomizing steam carbonyl compound should
With, it is characterised in that comprise the following steps:
The suction nozzle of one end of sampling tube with electronic smoke atomizer is tightly connected, the atomizing steam that described electronic smoke atomizer is discharged
Entered in described sampling tube by described suction nozzle again, and discharged by the other end in described sampling tube, now, described atomizing steam
In carbonyl compound with the derivatization reagent generation derivative reaction in described sampling tube thus be captured；
After sampling terminates, take out the silica gel particle in described sampling tube, in described silica gel particle, then add desorption solvent, with
After afterwards the solvent after desorbing being centrifuged 5-10min, supernatant use high performance liquid chromatograph-UV-detector detect,
Obtain the content of carbonyl compound in described electronic cigarette atomizing steam.
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Cited By (1)
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| CN112461612A (en) * | 2019-09-09 | 2021-03-09 | 斤技科技(北京)有限公司 | Multi-channel carbonyl compound sampler |
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Address after: 1b, building 6, saitu digital industrial plant, 137 Bulan Road, gankeng community, Jihua street, Shenzhen City, Guangdong Province Patentee after: Hengxin Yongji Technology (Shenzhen) Co.,Ltd. Patentee after: VISION EAST TECHNOLOGY (SHENZHEN) Co.,Ltd. Patentee after: HANGSEN INTERNATIONAL Group Ltd. Address before: 518112 501, 901, 1001, building 9, China Hisense innovation industry city, No. 3, ganliwu Road, Buji street, Longgang District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN HANGSEN STAR TECHNOLOGY Co.,Ltd. Patentee before: VISION EAST TECHNOLOGY (SHENZHEN) Co.,Ltd. Patentee before: HANGSEN INTERNATIONAL Group Ltd. |
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Effective date of registration: 20211116 Address after: Room 301, building 2, No. 1, Jinqi Road, Fenggang town, Dongguan City, Guangdong Province Patentee after: Hengxin Weiye Technology (Dongguan) Co.,Ltd. Address before: 518000 room 1b, building 6, saitu digital industrial plant, No. 137, Bulan Road, gankeng community, Jihua street, Shenzhen, Guangdong Patentee before: Hengxin Yongji Technology (Shenzhen) Co.,Ltd. Patentee before: VISION EAST TECHNOLOGY (SHENZHEN) Co.,Ltd. Patentee before: HANGSEN INTERNATIONAL Group Ltd. |