CN110967427B - Method for high-stability determination of ammonia content in cigarette mainstream smoke by adopting ion chromatography - Google Patents
Method for high-stability determination of ammonia content in cigarette mainstream smoke by adopting ion chromatography Download PDFInfo
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Abstract
The invention discloses a method for measuring the ammonia content in mainstream smoke of cigarettes by adopting ion chromatography with high stability, which comprises the following steps: s1, collecting total particulate matters and gaseous ammonia of main stream smoke of cigarettes; s2, extracting total particulate matters by using an extracting agent prepared from tobacco shred raw materials to obtain an extraction liquid, collecting gaseous ammonia by using dilute hydrochloric acid to obtain a collection liquid, diluting the mixed extraction liquid and the collection liquid in equal volumes to a constant volume, and filtering; and S3, performing ion chromatographic analysis on the filtrate to obtain an ion chromatogram in the cigarette sample, performing qualitative determination according to retention time, quantifying by using an external standard method, and deducting the ammonia content in the extracting agent to obtain the ammonia content in the mainstream smoke of the cigarette, wherein the extracting agent prepared from the cut tobacco raw material is used to improve the stability of an ammonia detection result.
Description
Technical Field
The invention relates to the field of smoke analysis, in particular to a method for measuring the ammonia content in main stream smoke of cigarettes with high stability by adopting an ion chromatography method.
Background
Ammonia is one of seven harmful components in main stream smoke of cigarettes, and the release amount of the ammonia directly influences the hazard index of products. At present, the research on the release amount of ammonia in mainstream smoke of conventional cigarettes is relatively more. The tobacco industry has established an industry standard method YC/T377-2010 for analyzing the ammonia content in mainstream smoke by ion exchange chromatography, but the ammonia content in the ammonia solution to be detected is unstable, and the total amount of ammonia in the extraction liquid can continuously rise, so that the accurate ammonia value is not favorably determined. The standard pretreatment method is revised, and the stability of the liquid to be detected is stabilized by injecting the sample under the low temperature condition, but the method has higher requirements on a sample injector, and can not control the precursor substance causing ammonia release in the extraction process to release ammonia.
Disclosure of Invention
In order to solve the problems, the invention provides a method for measuring the ammonia content in the mainstream smoke of cigarettes with high stability by adopting an ion chromatography, and an extracting agent prepared from tobacco shred raw materials is used, so that the stability of an ammonia detection result is improved, and the detection sensitivity is high.
The technical scheme for solving the problem is to provide a method for measuring the ammonia content in the mainstream smoke of cigarettes by adopting ion chromatography with high stability, which comprises the following steps:
s1, collecting total particulate matters and gaseous ammonia of main stream smoke of cigarettes;
s2, extracting the total particulate matter by using an extractant prepared from tobacco shred raw materials to obtain an extraction liquid, collecting gaseous ammonia by using dilute hydrochloric acid to obtain a collection liquid, diluting the mixed extraction liquid and the collection liquid with equal volumes to a constant volume, and filtering;
and S3, obtaining an ion chromatogram map in the cigarette sample by analyzing the filtrate through ion chromatography, quantifying by using an external standard method according to the qualitative retention time, and deducting the ammonia content in the extracting agent to obtain the ammonia content in the main stream smoke of the cigarette.
Preferably, the preparation steps of the extractant prepared from the cut tobacco raw material are as follows: heating the tobacco shreds sprayed with the glycerol at the temperature of 400 ℃ under the temperature of 300-.
Preferably, the chromatographic column for ion chromatographic analysis is CS16, the mobile phase is 0.045 mol/L methanesulfonic acid solution, the flow rate is 1.0 mL/min, the sample amount is 25 μ L, the column temperature is 30 ℃, the conductivity cell temperature is 35 ℃, and the suppressor current is 132 mA.
Preferably, the extraction time of S2 is 15-20min, and the extraction mode is ultrasonic oscillation extraction.
Preferably, the S1 total particulate matter is captured by a Cambridge filter, and the gaseous ammonia is captured by 10mmol/L diluted hydrochloric acid.
Preferably, the step S1 is preceded by the step of: balancing the cigarettes, wherein the temperature of the balancing condition is (22 +/-1) ° C, the relative humidity is (60 +/-3)%, and the balancing time is 48 h.
Preferably, the using amount of the glycerol is 10-20% of the mass of the cut tobacco.
Preferably, the dilute hydrochloric acid concentration is 10 mmol/L.
According to the scheme, the tobacco shreds are atomized by using the atomizing agent glycerol to release smoke, the extracting agent containing tobacco shred raw materials is obtained after the smoke is absorbed by dilute hydrochloric acid, the extracting agent is used for extracting total particulate matters of main stream smoke of a sample cigarette, 34 volatile organic matters in air in a tobacco shred storage room are mainly esters, aldehydes, ketones and the like, and since the glycerol can extract ketone substances in the tobacco shreds, on one hand, carbonyl of the ketone substances inhibits precursor substances of ammonia in cigarette smoke, namely unstable urotropine and other substances from being reversibly degraded into aldehyde ketone and ammonia, on the other hand, the carbonyl of the ketone substances can perform a Maillard reaction with stable amino in the smoke to play a role in anchoring ammonia, so that the measured result is more stable.
The invention has the following beneficial effects:
1. extracting by using an extracting agent prepared from tobacco shred raw materials, inhibiting the degradation of substances such as unstable ammonia precursor urotropine and the like of a detected object by using ketone substances of the tobacco shred or anchoring ammonia in cigarette smoke, improving the stability of ammonia detection liquid, and having good repeatability of detection results and high universality;
2. the content of ammonia in the sample solution is accurately and rapidly determined by using the ion chromatography, and the method is suitable for analyzing the ammonia release amount of the cigarette sample in a large scale;
3. the CS16 chromatographic column is adopted to measure the ammonia content in the mainstream smoke of the cigarette, and the detection sensitivity is high and the linear range is wide.
Drawings
FIG. 1 is an ion chromatography spectrum of example 1;
FIG. 2 is an ion chromatography profile of example 2;
FIG. 3 is an ion chromatography spectrum of example 3.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
Preparing an extracting agent containing tobacco shred raw materials: spraying 15% glycerol into 10g tobacco shred, heating tobacco shred at 300 deg.C, collecting flue gas with 100ml dilute hydrochloric acid solution with concentration of 10mmol/L, collecting flue gas with the obtained absorption solution with 40 ml dilute hydrochloric acid solution with concentration of 10mmol/L, diluting to volume of 200ml, and using as extractant.
Drawing a standard curve: using 1000 mug/mL ammonia standard solution as mother solution, diluting the mother solution with 10mmol/L diluted hydrochloric acid, wherein the dilution times are 2000 times, 1000 times, 500 times, 250 times and 125 times in sequence, using an ion chromatography analysis method with a chromatographic column of CS16 and a mobile phase of 0.045 mol/L methanesulfonic acid solution, the flow rate of 1.0 mL/min, the sample injection amount of 25 mug, the column temperature of 30 ℃, the conductivity cell temperature of 35 ℃, and the suppressor current of 132 mA to determine the peak area of a chromatogram, and drawing a standard curve by linear regression, wherein the standard curve equation is as follows: y =0.209X
And (3) sample determination: a commercially available cigarette sample A was equilibrated at (22. + -. 1) ° C and relative humidity (60. + -. 3)% for 48 hours, and then the length of the butt of the smoked cigarette was determined and marked, and 4 cigarettes were smoked.
Collecting total particulate matters of the mainstream smoke by using a Cambridge filter disc, and collecting gaseous ammonia by using diluted hydrochloric acid with the concentration of 20mL and 10mmol/L to obtain a collection liquid;
putting a Cambridge filter disc trapping main stream smoke of 4 cigarettes into a 50mL conical flask, adding 20mL of an extracting agent prepared from a tobacco shred raw material, then placing the conical flask on a speed-regulating oscillator for oscillation for 15 min, setting the frequency of the oscillator to be 160r/min, obtaining an extraction liquid, accurately transferring 5mL of the grain-phase extraction liquid and 5mL of the gas-phase trapping liquid into a 25mL volumetric flask, fixing the volume, shaking uniformly, and filtering with a 0.45-micrometer water-phase needle filter to be tested;
using ion chromatography conditions consistent with the standard curve, wherein a chromatographic column is CS16, a mobile phase is 0.045 mol/L methanesulfonic acid solution, the flow rate is 1.0 mL/min, the sample introduction amount is 25 mu L, the column temperature is 30 ℃, the conductivity cell temperature is 35 ℃, and the suppressor current is 132 mA, determining the peak time 7.407min and the peak area by using ion chromatography, and measuring the ammonia content according to the standard curve, taking 1/5 of the ammonia content in the extractant as a blank, and deducting the blank to obtain the ammonia content in the main stream smoke of the cigarette, as shown in figure 1.
The results of measuring the content of ammonia in the solution to be measured of ammonia at different times are shown in table 1, and it can be seen from the table that the content of ammonia measured by applying the method of the present invention is relatively stable without significant change, while the content of ammonia measured by using the original standard method YC/T377-2010 is greatly changed.
TABLE 1 EXAMPLE 1 test tobacco samples the results of ammonia content stability analysis (unit: μ g/cig) using the new and standard methods YC/T377-2010
Note that I' shows the change of the ammonia content measured by the method; "II" indicates the change in ammonia content measured using the standard method YC/T377-2010.
According to the method, the release amount of ammonia in the mainstream smoke of the cigarette A is analyzed, and the repeated determination is carried out for 5 times, as shown in the table 2, the result shows that the repeatability of the experimental method is better.
TABLE 2 repeatability results of the test methods (unit: μ g/cig)
Example 2
Preparing an extracting agent containing tobacco shred raw materials: after spraying 20% glycerol in 5g tobacco shred, heating tobacco shred at 400 deg.C and collecting flue gas with 100ml dilute hydrochloric acid solution with concentration of 10mmol/L, collecting flue gas with the obtained absorption liquid with 40 ml dilute hydrochloric acid solution with concentration of 10mmol/L, diluting to volume of 200ml, and using as extractant. Drawing a standard curve: using 1000 mug/mL ammonia standard solution as mother solution, diluting the mother solution with 10mmol/L diluted hydrochloric acid, wherein the dilution times are 2000 times, 1000 times, 500 times, 250 times and 125 times in sequence, using an ion chromatography analysis method with a chromatographic column of CS16 and a mobile phase of 0.045 mol/L methanesulfonic acid solution, the flow rate of 1.0 mL/min, the sample injection amount of 25 mug, the column temperature of 30 ℃, the conductivity cell temperature of 35 ℃, and the suppressor current of 132 mA to determine the peak area of a chromatogram, and drawing a standard curve by linear regression, wherein the standard curve equation is as follows: y =0.218X
And (3) sample determination: a commercially available cigarette sample C was equilibrated at (22. + -. 1) ° C and relative humidity (60. + -. 3)% for 48 hours, and then the length of the butt of the smoked cigarette was determined and marked, and 4 cigarettes were smoked.
Collecting total particulate matters of the mainstream smoke by using a Cambridge filter disc, and collecting gaseous ammonia by using diluted hydrochloric acid with the concentration of 20mL being 10mmol/L to obtain a collection liquid;
putting the Cambridge filter disc with the main stream smoke of 4 cigarettes in a 50mL conical flask, adding 20mL of an extracting agent prepared from a tobacco shred raw material, then placing the conical flask on a speed-regulating oscillator for oscillation for 20min, setting the frequency of the oscillator to be 160r/min, obtaining an extraction liquid, accurately transferring 5mL of the grain-phase extraction liquid and 5mL of the gas-phase trapping liquid into a 25mL volumetric flask for constant volume, shaking uniformly, and filtering with a 0.45-micrometer water-phase needle filter to be measured;
using ion chromatography conditions consistent with the standard curve, wherein a chromatographic column is CS16, a mobile phase is 0.045 mol/L methanesulfonic acid solution, the flow rate is 1.0 mL/min, the sample introduction amount is 25 mu L, the column temperature is 30 ℃, the conductivity cell temperature is 35 ℃, and the suppressor current is 132 mA, determining the peak time 7.413min and the peak area by using ion chromatography, and measuring the ammonia content according to the standard curve, taking 1/5 of the ammonia content in the extractant as a blank, and deducting the blank to obtain the ammonia content in the main stream smoke of the cigarette, as shown in FIG. 2.
Analyzing the ammonia content of the liquid to be detected at regular intervals, and inspecting whether the ammonia release amount is stable.
As can be seen from the table 3, the ammonia content of the solution to be measured can be stabilized in a certain time range by the fine cigarette C, so that the method has good universality.
TABLE 3 stability analysis results of ammonia release amount of fine cigarette C (unit: μ g/cig)
Example 3
Preparing an extracting agent containing tobacco shred raw materials: spraying 10% glycerol into 8g tobacco shred, heating tobacco shred at 350 deg.C, collecting flue gas with 100ml dilute hydrochloric acid solution with concentration of 10mmol/L, and diluting the obtained absorption liquid with 10mmol/L dilute hydrochloric acid to 500 ml as extractant prepared from tobacco shred raw material.
Drawing a standard curve: using 1000 mug/mL ammonia standard solution as mother liquor, using the dilute hydrochloric acid to dilute the mother liquor, wherein the dilution times are 2000 times, 1000 times, 500 times, 250 times and 125 times in sequence, using a chromatographic column CS16 and a methanesulfonic acid solution with a mobile phase of 0.045 mol/L, the flow rate is 1.0 mL/min, the sample injection amount is 25 muL, the column temperature is 30 ℃, the conductivity cell temperature is 35 ℃, and the suppressor current is 132 mA, and determining a peak area chromatogram by an ion chromatography, as shown in FIG. 3, using linear regression to draw a standard curve, wherein the standard curve equation is as follows: y =0.196X
And (3) sample determination: a commercially available cigarette sample A was equilibrated at (22. + -. 1) ° C and relative humidity (60. + -. 3)% for 48 hours, and then the length of the butt of the smoked cigarette was determined and marked, and 4 cigarettes were smoked.
Collecting total particulate matters of the mainstream smoke by using a Cambridge filter disc, and collecting gaseous ammonia by using diluted hydrochloric acid with the concentration of 20mL being 10mmol/L to obtain a collection liquid;
putting the Cambridge filter disc with the main stream smoke of 4 cigarettes trapped in a 50mL conical flask, adding 20mL of an extracting agent prepared from a tobacco shred raw material, then carrying out ultrasonic extraction for 15 min in the conical flask at an ultrasonic frequency of 3000HZ to obtain an extract, accurately transferring 5mL of the granular phase extract and 5mL of the gas phase trapping liquid into a 25mL volumetric flask for constant volume, shaking uniformly, and filtering with a 0.45-micrometer water phase needle filter to be detected;
using ion chromatography with the flow rate of 1.0 mL/min, the sample introduction amount of 25 muL, the column temperature of 30 ℃, the conductivity cell temperature of 35 ℃ and the suppressor current of 132 mA, determining the peak time of 7.403min and the peak area and fixing the volume, determining the ammonia content according to the standard curve, taking 1/5 of the ammonia content in the extractant as a blank, and deducting the ammonia content in the main stream smoke of the cigarette by using ion chromatography conditions with the same preparation standard curve, wherein the chromatography column is CS16 and the mobile phase is 0.045 mol/L methanesulfonic acid solution.
The ammonia content in the solution to be measured was analyzed at regular intervals, and whether the ammonia release amount was stable or not was examined, and compared with the results obtained in example 1, as can be seen from table 4, the method for measuring ammonia content was highly consistent, and the results were stable.
TABLE 4 Ammonia stability results
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (5)
1. A method for measuring the ammonia content in the mainstream smoke of cigarettes with high stability by adopting ion chromatography is characterized by comprising the following steps:
s1, collecting total particulate matters and gaseous ammonia of main stream smoke of cigarettes;
s2, extracting the total particulate matter by using an extractant prepared from tobacco shred raw materials to obtain an extraction liquid, collecting gaseous ammonia by using dilute hydrochloric acid to obtain a collection liquid, diluting the mixed extraction liquid and the collection liquid with equal volumes to a constant volume, and filtering;
s3, obtaining an ion chromatogram map in the cigarette sample by analyzing the filtrate through ion chromatography, quantifying by using an external standard method according to the qualitative retention time, and deducting the ammonia content in the extracting agent to obtain the ammonia content in the mainstream smoke of the cigarette; the preparation steps of the extractant prepared from the cut tobacco raw material are as follows: heating the tobacco shreds sprayed with the glycerol at 300 ℃, and collecting the smoke with dilute hydrochloric acid, diluting and fixing the volume to obtain an extracting agent prepared from the tobacco shreds; the using amount of the glycerol is 15% of the mass of the cut tobacco; the chromatographic column of the ion chromatographic analysis is CS16, the mobile phase is 0.045 mol/L methanesulfonic acid solution, the flow rate is 1.0 mL/min, the sample volume is 25 muL, the column temperature is 30 ℃, the conductivity cell temperature is 35 ℃, and the suppressor current is 132 mA.
2. The method for high-stability determination of ammonia content in cigarette mainstream smoke by ion chromatography according to claim 1, wherein the S2 extraction time is 15-20min, and the extraction mode is ultrasonic oscillation extraction.
3. The method for high-stability determination of the ammonia content in the mainstream smoke of cigarettes by using the ion chromatography as claimed in claim 1, wherein the S1 total particulate matters are captured by Cambridge filter discs, and the gaseous ammonia is captured by 10mmol/L diluted hydrochloric acid.
4. The method for highly stably measuring the ammonia content in the mainstream smoke of a cigarette by using ion chromatography according to claim 1, wherein the step of S1 is preceded by the steps of: balancing the cigarettes at the temperature of 22 +/-1 ℃ and the relative humidity of 60 +/-3% for 48 h.
5. The method for high-stability determination of ammonia content in cigarette mainstream smoke by ion chromatography according to claim 1, wherein the concentration of the dilute hydrochloric acid is 10 mmol/L.
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