CN104215723A - Method for determining contents of monomethylamine and monoethylamine in side-stream smoke gas of cigarette through ion chromatography - Google Patents
Method for determining contents of monomethylamine and monoethylamine in side-stream smoke gas of cigarette through ion chromatography Download PDFInfo
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Abstract
The invention discloses a method for determining the contents of monomethylamine and monoethylamine in a side-stream smoke gas of a cigarette through ion chromatography. The method includes following steps: capturing the monomethylamine and the monoethylamine, treating a smoke gas sample of a cigarette, preparing a stock solution and a standard operation solution, and respectively performing ion chromatographic analysis to supernatant liquids. By means of the method, accurate determination of the monomethylamine and the monoethylamine can be achieved and defects that a derivatization-gas chromatographic method, which is used for determining the monomethylamine and the monoethylamine in a main-stream smoke gas of the cigarette in the prior art, is complex in operations, needs a long time and much labor intensity and is difficult in accurate quantitation are overcome. The method is simple in pre-treatment, is accurate, is high in sensitivity and is good in repeatability. According to distributing situations of the monomethylamine and the monoethylamine in a gas phase and a granular phase in the side-stream smoke gas, the gas phase and the granular phase are respectively treated and detected individually so that the method is more reasonable theoretically and the distributing situations of the the monomethylamine and the monoethylamine in the gas phase and the granular phase are convenient to master.
Description
Technical field
The invention belongs to physical and chemical inspection technical field, be specifically related to the mensuration of organic amine in cigarette side-stream smoke.
Background technology
In result of combustion of tobacco process, nicotine or other alkaloidal thermal degradation all likely generate monomethyl amine and monoethyl amine, monomethyl amine, monoethyl amine have strong foul smell, stronger stimulation and corrosive attack is had to skin, eyes, the upper respiratory tract and lung, time poisoning, central nervous system is impaired, can cause tracheitis, bronchitis, pneumonia, even pulmonary edema, China specifies that the safe level of monomethyl amine in air is 5mg/m
3.The existence in cigarette smoke of monomethyl amine and monoethyl amine is except comparatively large on the impact of cigarette odor-absorbing, and its existence in side-stream smoke also exists negative effect to surrounding environment.
The report of current document to monomethyl amine and monoethyl amine focuses mostly at samples such as water sample, cosmetics, beverages, less to the mensuration report of its content in cigarette smoke.The method adopted mainly contains spectrophotometric method, liquid phase chromatography, vapor-phase chromatography, headspace gas chromatography, the chromatography of ions etc.Wherein spectrophotometric method disturbing factor is more, and reappearance is poor; Liquid phase chromatography and vapor-phase chromatography generally will through derivation process, complex operation and consuming time; In headspace gas chromatography, amine molecule very easily adsorbs wall, and sample size is difficult to accurate control.
Summary of the invention
The invention provides one with methyl sulfonic acid for mobile phase Gradient elution, with 0.01mol/L hydrochloric acid solution for absorbing liquid, the method for monomethyl amine and monoethyl amine in chromatography of ions rapid and accurate determination cigarette side-stream smoke, the method comprises the following steps:
The trapping of monomethyl amine and monoethyl amine in A, side-stream smoke: after cigarette sample is balanced 48h in 22 DEG C ± 1 DEG C environment with relative humidity 60% ± 2%, select average weight for ± 0.02g/and average resistance to suction be ± cigarette that 49Pa/ props up is for testing cigarette, trap the granule phase substance of side-stream smoke with fish tail cover and glass fiber filter, the absorption bottles that employing two is connected simultaneously collect absorbing liquid absorb the gas gas-phase objects in side-stream smoke successively with the watery hydrochloric acid of the flow velocity 0.01mol/L of 3000mL/min after;
B, blank assay: get identical cigarette, do not lighting under state, often props up and carry out the average mouth number suction of correspondence, obtains laboratory room air blank and filter disc blank sample;
C, cigarette smoke sample preparation: a, side stream gas phases (fish tail cover+absorption bottle): trapping is had in the fish tail cover inwall 0.01mol/L hydrochloric acid solution drip washing container of gas gas-phase objects, again by after in two gas absorption bottles, absorbing liquid is transferred to said vesse, use hydrochloric acid solution washing absorption bottle and the side-stream smoke contact portion of 0.01mol/L respectively, cleansing solution is proceeded to said vesse in the lump, shake up after being settled to scale with hydrochloric acid solution again, pipette supernatant liquor after leaving standstill and treat ion chromatography; B, granule phase substance (filter disc): aspirated after cigarette terminates, take out glass fiber filter, after drip catcher inwall filter disc is cleaned, this filter disc and glass fiber filter are together put into Erlenmeyer flask, add the hydrochloric acid solution of 0.01mol/L, pipette supernatant liquor after ultrasonic extraction 50min, after 0.22 μm of aqueous phase membrane filtration, collect filtrate and treat ion chromatography;
D, the storing solution of monomethyl amine and monoethyl amine and the preparation of standard working solution: accurately take 0.1g40% mass concentration monomethylamine aqueous solution respectively, the monoethyl amine aqueous solution of 0.06g65% ~ 70% mass concentration is in container, after being settled to scale with 0.01mol/L hydrochloric acid solution, be mixed with monomethyl amine, the hybrid standard storing solution of monoethyl amine, then standard reserving solution described in stepwise dilution, be mixed with concentration and be respectively 0.02, 0.04, 0.08, 0.2, 0.4, 0.8, after the series standard working solution of 2.0 μ g/mL, the linear equation coefficient R of monomethyl amine ion and monoethyl amine ion is obtained through ion chromatography
2be 0.9999,
E, the supernatant liquor of above-mentioned a, b step is carried out ion chromatography respectively, chromatography of ions condition: chromatographic column: CS16 (4 × 250 mm) separating column, CGl6 (4 × 50 mm) guard column; Electric conductivity detector, wears peace CSRS ULTRA-II (4 mm) rejector; Mobile phase: 10mmol/L methyl sulfonic acid, Gradient elution, elution time is 40min; Flow velocity: 1.0 mL/min; Sample size: 25uL; Column temperature: 60 DEG C; Autosynthesis rejector electric current: 39mA.
By the side-stream smoke grain obtained after above-mentioned ion chromatography mutually in and in gas phase the content of monomethyl amine and monoethyl amine substitute into following formula (1) respectively and formula (2) calculates, then the total amount of monomethyl amine in side-stream smoke and monoethyl amine is substituted into the content that formula (3) gets final product monomethyl amine and monoethyl amine in rapid and accurate determination cigarette side-stream smoke.
In above formula: M
1---the determinand content in cigarette side-stream smoke gas phase, unit is that microgram is often propped up (μ g/ props up);
C
1---the mensuration concentration of determinand ion in gas phase liquid to be measured, unit is micrograms per millilitre (μ g/mL);
C
01---the mensuration concentration of determinand ion in gas phase blank solution, unit is micrograms per millilitre (μ g/mL);
M
2---cigarette side-stream smoke grain mutually in determinand content, unit is that microgram is often propped up (μ g/ props up);
C
2---the mensuration concentration of determinand ion in grain liquid mutually to be measured, unit is micrograms per millilitre (μ g/mL);
C
02---the mensuration concentration of determinand ion in grain phase blank solution, unit is micrograms per millilitre (μ g/mL);
M---determinand molecule formula weight, monomethyl amine is 31, and monoethyl amine is 45;
M---the determinand content in cigarette side-stream smoke, unit is that microgram is often propped up (μ g/ props up);
N---the number of suction cigarette, unit:.
Experimental result requires that being accurate to 0.1 μ g/ props up;
the technical progress that the present invention obtains:
Owing to adopting technique scheme of the present invention, the technical progress that the present invention obtains is:
1, the present invention adopts the chromatography of ions to achieve Accurate Determining to the monomethyl amine in cigarette side-stream smoke and monoethyl amine, overcome the complex operation that derivatization-vapor-phase chromatography that prior art adopts the mensuration of monomethyl amine in cigarette mainstream flue gas and monoethyl amine exists, waste time and energy, be difficult to the drawback of accurate quantitative analysis, Comparatively speaking, the chromatography of ions of the present invention has the advantages such as pre-treatment is simple, accurate, highly sensitive, reproducible, achieves the Accurate Determining to monomethyl amine in cigarette side-stream smoke and monoethyl amine.
2, in the present invention, the linear concentration scope of monomethyl amine and monoethyl amine is 0.02 ~ 2.0 μ g/mL, and the range of linearity is wider, linear equation coefficient R
2be 0.9999, linearly better.And actual sample gas phase and grain mutually in the concentration range of monomethyl amine be about 0.1 ~ 1.0 μ g/mL, the concentration range of monoethyl amine is about 0.05 ~ 0.5 μ g/mL, thus the mensuration linearly meeting actual sample completely of the present invention.
3, in the present invention, in cigarette side-stream smoke gas phase, the detectability of monomethyl amine and monoethyl amine is respectively that 0.25 μ g/ props up, 0.28 μ g/ props up; Grain mutually in the detectability of monomethyl amine and monoethyl amine be respectively that 0.038 μ g/ props up, 0.054 μ g/ props up, far below actual sample gas phase and grain mutually in the measured value of monomethyl amine and monoethyl amine, thus can realize the accurate quantitative analysis to monomethyl amine and monoethyl amine.
4, in the present invention, the recovery of monomethyl amine is between 80.7% ~ 102.9%, and the recovery of monoethyl amine is between 85.1% ~ 102.1%, and the recovery is better, illustrates that accuracy of the present invention is higher.The replicate determination 5 times under identical conditions of same cigarette sample, the precision (RSD) of the monomethyl amine calculated and monoethyl amine is all less than 3%, the present invention's repeatability is described better.
5, the present invention is according to monomethyl amine in side-stream smoke and the monoethyl amine distribution situation in gas phase and grain mutually two, and gas phase and grain are separately processed detection mutually, more reasonable in theory, and be convenient to grasp monomethyl amine and monoethyl amine gas phase and grain mutually in distribution situation.
Accompanying drawing explanation
Fig. 1 is side-stream smoke capturing device schematic diagram of the present invention.
Fig. 2 is monomethyl amine and monoethyl amine standard model chromatography of ions figure in cigarette side-stream smoke.
Fig. 3 is typical sample chromatography of ions figure.
Fig. 4 is the effect diagram of methyl sulfonic acid concentrations to determinand degree of separation.
Fig. 5 is the effect diagram of column temperature to determinand degree of separation.
Fig. 6 is ultrasonic time to the effect diagram of monomethyl amine in granule phase substance and monoethyl amine content.
Fig. 7 is monomethyl amine and monoethyl amine content changing trend diagram in time in liquid to be measured.
Embodiment
The present embodiment key instrument: adopt the five duct effluent smoking machines that German Borg.waldt.KC company as shown in Figure 1 produces, wherein connect main flume drip catcher 5 bottom fish tail cover 1, installing cambridge filter in drip catcher 5, drip catcher 5 inlet end passes into main flume 6, fish tail cover 1 top connects effluent Fume collector 2, side-stream smoke drip catcher 2 endpiece serial connection gas absorption bottle 3,4; U.S. Dai An company IC-3000 ion chromatograph, joins electric conductivity detector and gradient elution pump; The KQ-500 type ultrasonic washing instrument that Kunshan Ultrasonic Instruments Co., Ltd. produces; The 0.0001g AB204-S type electronic balance that Mettler Toledo company of Switzerland produces and the Elix Milli-Q ultrapure water machine that MILLIPORE SAS company of the U.S. produces.
Main agents and material: analyze single methylamine, 40% aqueous solution, analyzes single ethamine 65% ~ 70% aqueous solution, top grade pure hydrochloric acid; Φ 44 cambridge filter; 80ml gas absorption bottle; Purchased from 10 kinds of cigarette samples of local market; Absorbing liquid is the aqueous hydrochloric acid solution of 0.01mol/L.
Realize the method for monomethyl amine and monoethyl amine content in ion-chromatographic determination cigarette side-stream smoke of the present invention, comprise the following steps:
The trapping of monomethyl amine and monoethyl amine in A, side-stream smoke: after cigarette sample is balanced 48h in 22 DEG C ± 1 DEG C environment with relative humidity 60% ± 2%, select average weight for ± 0.02g/and average resistance to suction be ± cigarette that 49Pa/ props up is for testing cigarette, with the granule phase substance of fish tail cover and glass fiber filter trapping side-stream smoke, adopt simultaneously two series connection respectively add the gas gas-phase objects having the hydrochloric acid solution of 30mL0.01mol/L to absorb in side-stream smoke successively with the watery hydrochloric acid of the flow velocity 0.01mol/L of 3000mL/min as absorbing liquid after collect absorbing liquid; Had a suck of according to every 60 seconds, every mouthful of puff duration 2s, every mouthful of pumping volume 35ml, then cigarette side-stream smoke granule phase substance is collected with the cambridge filter of Φ 44mm, on five duct effluent smoking machines, four cigarette are aspirated in each duct, after cigarette smoking terminates, fish tail cover, side-stream smoke drip catcher and two absorption bottles of connecting are taken out in suction 2 mouthfuls afterwards, carry out sample pre-treatments immediately;
B, blank assay: get identical cigarette, do not light, often prop up and carry out the average mouth number suction of correspondence, obtains, at the laboratory room air blank of not lighting under state and filter disc blank sample, carrying out blank deduction after process in last measurement result;
C, cigarette smoke sample preparation: a, side stream gas phases (fish tail cover+absorption bottle): fish tail cover inwall 60mL concentration is that the hydrochloric acid solution drip washing of 0.01mol/L is in 200mL volumetric flask, again absorbing liquid in two gas absorption bottles is transferred to after in above-mentioned 200mL volumetric flask, be hydrochloric acid solution washing absorption bottle and the side-stream smoke contact portion of 0.01mol/L respectively by 30mL concentration, after each absorption bottle respectively washs 2 times ~ 3 times, cleansing solution is proceeded in the lump in 200mL volumetric flask, shake up after being settled to scale with hcl as extraction agent solution again, pipette 1mL supernatant liquor after leaving standstill 2min and treat ion chromatography, b, granule phase substance (filter disc): aspirated after cigarette terminates, take out glass fiber filter, clean 1/4th filter discs of drip catcher inwall are wiped clean, this filter disc and glass fiber filter are together put into 100mL Erlenmeyer flask, accurately add the hydrochloric acid solution that 30mL concentration is 0.01mol/L, pipette about 2mL supernatant liquor after ultrasonic extraction 50min, after 0.22 μm of aqueous phase membrane filtration, filtrate treats ion chromatography,
D, the storing solution of monomethyl amine and monoethyl amine and the preparation of standard working solution: accurately take 0.1g40% mass concentration monomethylamine aqueous solution respectively, the monoethyl amine aqueous solution of 0.06g65% ~ 70% mass concentration is in 100mL volumetric flask, after being settled to scale with 0.01mol/L hydrochloric acid solution, be mixed with monomethyl amine, the hybrid standard storing solution of monoethyl amine, then standard reserving solution described in stepwise dilution, be mixed with concentration and be respectively 0.02, 0.04, 0.08, 0.2, 0.4, 0.8, after the series standard working solution of 2.0 μ g/mL, the linear equation coefficient R of monomethyl amine ion and monoethyl amine ion is obtained through ion chromatography
2be 0.9999,
E, the supernatant liquor of above-mentioned a, b step is carried out ion chromatography respectively, chromatography of ions condition: chromatographic column: CS16 (4 × 250 mm) separating column, CGl6 (4 × 50 mm) guard column; Electric conductivity detector, wears peace CSRS ULTRA-II (4 mm) rejector; Mobile phase: 10mmol/L methyl sulfonic acid, Gradient elution, elution time is 40min; Flow velocity: 1.0 mL/min; Sample size: 25uL; Column temperature: 60 DEG C; Autosynthesis rejector electric current: 39mA.
Obtain monomethyl amine as shown in Figure 2 and monoethyl amine standard model chromatography of ions figure and typical sample chromatography of ions figure as shown in Figure 3, in Fig. 2, a represents monomethyl amine ion, and b represents monoethyl amine ion; In Fig. 3, c represents monomethyl amine ion, and d represents monoethyl amine ion.
By the side-stream smoke grain obtained after above-mentioned ion chromatography mutually in and in gas phase the content of monomethyl amine and monoethyl amine substitute into following formula (1) respectively and formula (2) calculates, then the total amount of monomethyl amine in side-stream smoke and monoethyl amine is substituted into the content that formula (3) gets final product monomethyl amine and monoethyl amine in rapid and accurate determination cigarette side-stream smoke.
In above formula: M
1---the determinand content in cigarette side-stream smoke gas phase, unit is that microgram is often propped up (μ g/ props up);
C
1---the mensuration concentration of determinand ion in gas phase liquid to be measured, unit is micrograms per millilitre (μ g/mL);
C
01---the mensuration concentration of determinand ion in gas phase blank solution, unit is micrograms per millilitre (μ g/mL);
M
2---cigarette side-stream smoke grain mutually in determinand content, unit is that microgram is often propped up (μ g/ props up);
C
2---the mensuration concentration of determinand ion in grain liquid mutually to be measured, unit is micrograms per millilitre (μ g/mL);
C
02---the mensuration concentration of determinand ion in grain phase blank solution, unit is micrograms per millilitre (μ g/mL);
M---determinand molecule formula weight, monomethyl amine is 31, and monoethyl amine is 45;
M---the determinand content in cigarette side-stream smoke, unit is that microgram is often propped up (μ g/ props up).
N---the number of suction cigarette, unit:.
Experimental result requires that being accurate to 0.1 μ g/ props up.
Have studied with methyl sulfonic acid for mobile phase Gradient elution herein, with the hydrochloric acid solution of 0.01mol/L for absorbing liquid, the monomethyl amine in chromatography of ions Fast Measurement cigarette side-stream smoke and monoethyl amine, and the method condition is optimized and is evaluated.
Condition determination of the present invention is analyzed
1, the selection of ion chromatographic column
Because in cigarette smoke, ammonium ion, monomethyl amine ion, monoethyl amine ion interfere with each other; for three is separated completely; select CS12 (4 × 250mm) separating column, CGl2 (4 × 50mm) guard column and CS16 (4 × 250mm) separating column, CGl6 (4 × 50 mm) guard column two kinds of chromatographic columns, found that CS16 post separating effect is better.
2, the selection of methyl sulfonic acid concentrations
Methyl sulfonic acid is selected to be mobile phase wash-out test substance, can the concentration of mobile phase particularly crucial to be separated determinand completely, for by complete to the ammonium ion in cigarette side-stream smoke, monomethyl amine ion and monoethyl amine ion isolation, have selected 10mmol/L, 20 mmol/L, 30 mmol/L methyl sulfonic acid Gradient elutions, as shown in Figure 4, wherein a
1represent monomethyl amine ion, b1 represents monoethyl amine ion.As shown in Figure 4, during 10mmol/L methyl sulfonic acid Gradient elution, ammonium ion, monomethyl amine ion can be separated completely with monoethyl amine ion.
3, the selection of column temperature
Column temperature all has impact to the degree of separation, retention time, post pressure etc. at spectrum peak of looking for be measured, test the separation case of each determinand when column temperature is respectively 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, as shown in Figure 5, wherein c1 represents monomethyl amine ion, d1 represents monoethyl amine ion, when Fig. 5 shows 60 DEG C, the separating effect of each determinand is best, thus selects column temperature to be 60 DEG C in embodiment.
4, the selection of flow velocity
Flow rate of mobile phase has influence on appearance time, the degree of separation of ion, and when flow rate of mobile phase is too high, interionic degree of separation is deteriorated, and flow rate of mobile phase is too low, and minute is long.Have selected 0.5 by experiment, 0.8,1.0, the flow rate of mobile phase of 1.2mL/min, comprehensively analyze degree of separation and retention time, the present invention selects the flow velocity of comparatively suitable 1.0 mL/min.
5, the selection of absorbing liquid concentration
For guaranteeing monomethyl amine in cigarette side-stream smoke gas gas-phase objects and granule phase substance, monoethyl amine is completely absorbed and extracts, test have selected 0.005,0.01, the hydrochloric acid of 0.02mol/L tri-kinds of variable concentrations is as absorbing liquid and extract, added absorbing liquid and extract volume are 30mL, know from table 1 result that 0.01mol/L aqueous hydrochloric acid solution can reach satisfied.
Table 1 absorbing liquid concentration is on the impact of determinand content
6, the selection of absorption bottle series connection number
For guaranteeing the monomethyl amine in components in cigarette smoke gas phase thing, monoethyl amine is completely absorbed, connecting 3 after drip catcher, 30mL concentration is housed respectively is that the absorption bottle of 0.01mol/L aqueous hydrochloric acid solution traps gas phase composition, after aspirating 4 cigarette, solution in three absorption bottles is shaken up, cross 0.22 μm of aqueous phase filter membrane and carry out ion chromatography, by analyzing the absorption efficiency of three absorption bottles, found that, preposition absorption bottle, in mid-absorption bottle and rearmounted absorption bottle, the concentration of monomethylamine is respectively 0.339, 0.0513, 0.0066 μ g/mL, the ratio accounting for total concentration is respectively 85.4%, 12.9%, 1.7%, in three absorption bottles, the concentration of monoethyl amine is respectively 0.157,0.0144,0 μ g/mL, accounts for 91.6% of total concentration ratio, 8.4%, 0% respectively.Data show in cigarette side-stream smoke more than 98% monomethyl amine and monoethyl amine all absorbed by the first two absorption bottle, therefore the gas gas-phase objects of the absorption bottle trapping side-stream smoke of test selection two series connection, respectively in absorption bottle loads 30mL absorbing liquid.
7, the selection of mode and extraction time is extracted
Test have selected ultrasonic and vibration two kinds of extraction modes, for 1# cigarette, after the analysis of oscillation extraction 50min sample introduction, the content of monomethyl amine, monoethyl amine is respectively that 8.4 μ g/ prop up, 1.6 μ g/ prop up, after the analysis of ultrasonic extraction 50min sample introduction, the content of monomethyl amine, monoethyl amine is respectively that 9.1 μ g/ prop up, 1.8 μ g/ prop up, and ultrasonic extraction rate is a little more than oscillation extraction.Ultrasonic extraction mode is selected in test, is to optimize the ultrasonic extraction time, test have selected 20,30,40,50,60min different extraction time time determinand extraction efficiency, as shown in Figure 6, wherein "
" represent monomethyl amine, "
" represent monoethyl amine.As shown in Figure 6, after extraction time reaches 50min, the determinand content in extract does not change substantially, and therefore extraction time is chosen as 50min.
8, the stability of solution to be measured
Determinand in cigarette smoke is subject to the impact of environment and sample substrate itself, and along with the prolongation of standing time, the content of determinand increases gradually, with sample liquid to be measured for analytic target, place 0h, 1h, 2h, 4h, 8h, 12h, 16h, 24h and 48h respectively, testing result is shown in accompanying drawing 7, wherein "
" represent monomethyl amine, "
" represent monoethyl amine.Can find from Fig. 7, in 12h, the measured value change of monomethyl amine and monoethyl amine is all within 5%, the content of monomethyl amine and monoethyl amine increases gradually afterwards, after liquid to be measured places 48h, the content of monomethyl amine and monoethyl amine increases by 10.6% and 14.6% respectively, and therefore testing requirements sample must complete detection by 12h after cigarette smoking completes.
9, standard working curve, detectability and quantitative limit
The series standard working solution concentration prepared being respectively 0.02,0.04,0.08,0.2,0.4,0.8,2.0 μ g/mL carries out ion chromatography, take target concentration as horizontal ordinate, with determinand peak area in chromatogram for ordinate, carry out regretional analysis, obtain the linear equation of determinand.The multiple sample introduction of minimum standard specimen solution weight 10 times, calculate the standard deviation of measured value, using 3 times of standard deviation scaling results as the detection limit of method, using 10 times of standard deviation scaling results as the quantitative limit of method, data see the following form 2.
The linear equation of table 2 method, related coefficient, detectability and quantitative limit
10, the recovery and repeatability
Grain phase (filter disc) sample segment recovery of standard addition: the standard solution adding 3 variable concentrations on the glass fiber filter aspirated respectively by basic, normal, high concentration, add 30mL0.01mol/L hydrochloric acid solution ultrasonic extraction 50min, after getting supernatant liquor filtering membrane after leaving standstill, carry out ion chromatography; Gas phase portion sample recovery of standard addition: in the 200mL volumetric flask proceeding to fish tail cover leacheate and absorption bottle leacheate, add the standard solution of 3 variable concentrations respectively by basic, normal, high concentration, shake up, solution filtering membrane, carry out ion chromatography, recovery test the results are shown in following table 3.As shown in Table 3, the recovery of monomethyl amine is between 80.7% ~ 102.9%, and the recovery of monoethyl amine is between 85.1% ~ 102.1%, and the recovery is better, illustrates that the method accuracy is higher.The replicate determination 5 times under identical conditions of same cigarette sample, calculate the relative standard deviation (RSD) of 5 parallel determinations, measurement result sees the following form 3.Result display in table 3, the precision RSD of monomethyl amine and monoethyl amine is all less than 3%, this method repeatability is described better.
The recovery of table 3 method and precision (RSD)
11, the content of monomethyl amine and monoethyl amine in part cigarette side-stream smoke
Adopt the inventive method to detect the monomethyl amine in the sample of 10 kinds of cigarettes types, different tar content and monoethyl amine content, the results are shown in Table 4.Result shows: the monomethyl amine 1. in side-stream smoke and monoethyl amine are mainly present in gas phase portion, accounts for about 70% of total content; 2., in 10 samples, in 2 blended type cigarettes, the content of monomethyl amine and monoethyl amine is all higher than all the other 8 Virginian-type cigarettes.
Table 4 sample detection result (μ g/ props up)
Claims (1)
1. the method for monomethyl amine, monoethyl amine content in an ion-chromatographic determination cigarette side-stream smoke:
The trapping of monomethyl amine and monoethyl amine in A, side-stream smoke: after cigarette sample is balanced 48h in 22 DEG C ± 1 DEG C environment with relative humidity 60% ± 2%, select average weight for ± 0.02g/and average resistance to suction be ± cigarette that 49Pa/ props up is for testing cigarette, trap the granule phase substance of side-stream smoke with fish tail cover and glass fiber filter, the absorption bottles that employing two is connected simultaneously collect absorbing liquid absorb the gas gas-phase objects in side-stream smoke successively with the watery hydrochloric acid of the flow velocity 0.01mol/L of 3000mL/min after;
B, blank assay: get identical cigarette, do not lighting under state, often props up and carry out the average mouth number suction of correspondence, obtains laboratory room air blank and filter disc blank sample;
C, cigarette smoke sample preparation: a, side stream gas phases (fish tail cover+absorption bottle): trapping is had in the fish tail cover inwall 0.01mol/L hydrochloric acid solution drip washing container of gas gas-phase objects, again by after in two gas absorption bottles, absorbing liquid is transferred to said vesse, use hydrochloric acid solution washing absorption bottle and the side-stream smoke contact portion of 0.01Mmol/L respectively, cleansing solution is proceeded to said vesse in the lump, shake up after being settled to scale with hcl as extraction agent solution again, stirring pipettes supernatant liquor after leaving standstill and treats ion chromatography; B, granule phase substance (filter disc): aspirated after cigarette terminates, take out glass fiber filter, after drip catcher inwall filter disc is cleaned, this filter disc and glass fiber filter are together put into Erlenmeyer flask, add the hydrochloric acid solution of 0.01mol/L, pipette supernatant liquor after ultrasonic extraction 50min, after 0.22 μm of aqueous phase membrane filtration, collect filtrate and treat ion chromatography;
D, the storing solution of monomethyl amine and monoethyl amine and the preparation of standard working solution: accurately take 0.1g40% mass concentration monomethylamine aqueous solution respectively, the monoethyl amine aqueous solution of 0.06g65% ~ 70% mass concentration is in container, after being settled to scale with 0.01mol/L hydrochloric acid solution, be mixed with monomethyl amine, the hybrid standard storing solution of monoethyl amine, then standard reserving solution described in stepwise dilution, be mixed with concentration and be respectively 0.02, 0.04, 0.08, 0.2, 0.4, 0.8, after the series standard working solution of 2.0 μ g/mL, the linear equation coefficient R of monomethyl amine ion and monoethyl amine ion is obtained through ion chromatography
2be 0.9999,
E, the supernatant liquor of above-mentioned a, b step is carried out ion chromatography respectively, chromatography of ions condition: chromatographic column: CS16 (4 × 250 mm) separating column, CGl6 (4 × 50 mm) guard column; Electric conductivity detector, wears peace CSRS ULTRA-II (4 mm) rejector; Mobile phase: 10mmol/L methyl sulfonic acid, Gradient elution, elution time is 40min; Flow velocity: 1.0 mL/min; Sample size: 25uL; Column temperature: 60 DEG C; Autosynthesis rejector electric current: 39mA.
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| CN110261530A (en) * | 2019-07-25 | 2019-09-20 | 日照海关综合技术服务中心 | 20 kinds of organic amines, biogenic amine and cation method for measuring simultaneously in a kind of fruit drink |
| CN111239320A (en) * | 2019-09-29 | 2020-06-05 | 台州学院 | Method for detecting volatile organic amine compounds |
| CN114689715A (en) * | 2020-12-29 | 2022-07-01 | 北京海浈医药科技有限公司 | Method for detecting content of trimethylamine or trimethylamine salt |
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| CN106596196A (en) * | 2016-12-15 | 2017-04-26 | 西安交通大学 | Elevation-type cigarette side-stream smoke aerosol rapid collecting hood and detection method thereof |
| CN106596196B (en) * | 2016-12-15 | 2018-12-07 | 西安交通大学 | A kind of lift cigarette side flow smoke aerosol Quick Acquisition cover and its detection method |
| CN110261530A (en) * | 2019-07-25 | 2019-09-20 | 日照海关综合技术服务中心 | 20 kinds of organic amines, biogenic amine and cation method for measuring simultaneously in a kind of fruit drink |
| CN110261530B (en) * | 2019-07-25 | 2021-06-08 | 日照海关综合技术服务中心 | Method for simultaneously determining 20 organic amines, biogenic amines and cations in fruit juice beverage |
| CN111239320A (en) * | 2019-09-29 | 2020-06-05 | 台州学院 | Method for detecting volatile organic amine compounds |
| CN114689715A (en) * | 2020-12-29 | 2022-07-01 | 北京海浈医药科技有限公司 | Method for detecting content of trimethylamine or trimethylamine salt |
| CN114689715B (en) * | 2020-12-29 | 2024-01-16 | 北京海浈医药科技有限公司 | Method for detecting trimethylamine or trimethylamine salt content |
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| CN104215723B (en) | 2016-10-05 |
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