CN113310971A - Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar - Google Patents

Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar Download PDF

Info

Publication number
CN113310971A
CN113310971A CN202110374014.XA CN202110374014A CN113310971A CN 113310971 A CN113310971 A CN 113310971A CN 202110374014 A CN202110374014 A CN 202110374014A CN 113310971 A CN113310971 A CN 113310971A
Authority
CN
China
Prior art keywords
formaldehyde
solution
acetaldehyde
total content
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.)
Pending
Application number
CN202110374014.XA
Other languages
Chinese (zh)
Inventor
王春琼
陈丹
曾彦波
张轲
蔡洁云
彭丽娟
张晓伟
孙浩巍
龙杰
曾天宝
杨艺敏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yunnan tobacco quality supervision and inspection station
Original Assignee
Yunnan tobacco quality supervision and inspection station
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Yunnan tobacco quality supervision and inspection station filed Critical Yunnan tobacco quality supervision and inspection station
Priority to CN202110374014.XA priority Critical patent/CN113310971A/en
Publication of CN113310971A publication Critical patent/CN113310971A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

Abstract

The invention discloses a continuous flow method for measuring the total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar. Taking electronic cigarette tobacco tar, using 20% ethanol water solution to fix the volume as a sample, respectively preparing a phenol reagent, an ammonium ferric sulfate reagent and a cleaning solution, and measuring the total content of formaldehyde and acetaldehyde at a wavelength of 630nm by using a continuous flow analyzer. The method has the advantages of simple and convenient operation, simple pretreatment, high analysis speed, strong anti-interference performance, accurate result, high precision, good repeatability and stability, wide detectable concentration range, low detection limit and quantification limit, and is particularly suitable for detecting the total content of formaldehyde and acetaldehyde in a large batch of electronic cigarette tobacco tar samples.

Description

Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar
Technical Field
The invention belongs to the technical field of novel tobacco physical and chemical index detection, and particularly relates to a method for quickly and accurately determining the total content of formaldehyde and acetaldehyde in tobacco tar of an electronic cigarette by using a continuous flow analyzer.
Background
Formaldehyde is a moderately toxic substance, LD50800mg/Kg (rat is taken orally), severe damage to bronchus and lung can occur after 5-10min of inhalation, the oral lethal dose is about 10-20mL, and the medicine has high toxicity and carcinogenicity, and is classified as a class I human carcinogen by the international cancer research institution. Acetaldehyde can stimulate skin and mucous membrane, the vapor of the acetaldehyde is corrosive to respiratory tract, the high-concentration acetaldehyde has sensitization, mutagenicity and teratogenicity, the acetaldehyde can cause DNA damage of human bodies and promote the formation of liver diseases, and the acetaldehyde is listed in II carcinogens by the international cancer research organization of the world health organization.
In recent years, with the increasing of global smoking control, the sales of traditional cigarettes in developed countries has a certain declining trend, and the sales of electronic cigarettes in the world is rapidly increasing. An electronic cigarette, also called an electric atomization cigarette, is an electronic device that transmits nicotine to a respiratory system by an electronic heating means. The electronic cigarette tobacco tar refers to liquid or gel used for generating aerosol by electronic cigarettes and used for being sucked by consumers, and most of the electronic cigarette tobacco tar is a mixture composed of propylene glycol, glycerin, nicotine, various essences for improving mouthfeel and the like. The electronic cigarette is used as a novel tobacco product, the content levels of formaldehyde and acetaldehyde in the cigarette oil of the electronic cigarette are mastered, the safety quality monitoring of the electronic cigarette product is facilitated to be improved, and the electronic cigarette has important significance for protecting the health and safety of consumers and improving the quality of the electronic cigarette.
At present, the detection of formaldehyde and acetaldehyde mostly focuses on cigarette auxiliary materials such as cigarette wrapping paper, cigarette blasting beads, cigarette water-based glue, cigarette acetate fiber filter rods and the like, for example, after formaldehyde and acetaldehyde are derivatized by 2, 4-dinitrophenylhydrazine, people such as joyous and the like, the formaldehyde and the acetaldehyde in the cigarette wrapping paper are determined by adopting an ultra-high performance liquid chromatography; liuxin et al are also derivatized with 2, 4-dinitrophenylhydrazine, and formaldehyde and acetaldehyde in the exploded beads are determined by high performance liquid chromatography; zhang jin Qing et al established a derivatization-headspace gas chromatography method for measuring formaldehyde, acetaldehyde and acetone in water-based adhesive for cigarettes.
Although the chromatographic detection method has made many important advances in tobacco detection, there are many defects: the instrument and equipment are expensive, the detection cost is high, the detection period is long, and the operation of professionals is needed, so that the popularization is difficult, and the requirement of large-scale detection is difficult to meet. And the pretreatment is very complicated, a series of pretreatment operations such as solvent extraction, centrifugal removal of precipitates, filtration and derivatization are needed to obtain an analysis test solution, and some analysis test solutions are also needed to be enriched or purified by solid-phase extraction, and operation errors are easily introduced in the sample transfer process, so that the detection accuracy is influenced.
Compared with the method, the continuous flow analyzer is cheap in equipment, low in maintenance cost, simple in pretreatment, simple and convenient in operation on a machine, high in detection speed, accurate in quantification, good in reproducibility and the like, organic reagents are not needed in detection, the environment is more friendly, the detection of chemical components such as water-soluble sugar, total plant alkaloid, total nitrogen, total volatile acid, starch, free nicotine and the like in tobacco and tobacco products is carried out in the tobacco industry in China since the continuous flow analyzer is introduced in the eighties of the last century, the detection of chemical components such as chlorine, potassium, nitrate and the like in cigarette paper is carried out by adopting the continuous flow analyzer, but the report of using the continuous flow analyzer to detect the total content of formaldehyde and acetaldehyde in the electronic cigarette oil is not seen at present.
Disclosure of Invention
The invention aims to provide a method for rapidly, simply and accurately measuring the total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar aiming at the defects of the prior art.
The purpose of the invention is realized by the following technical scheme.
All percentages used herein are volume percentages unless otherwise indicated.
A continuous flow method for measuring the total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar comprises the following steps:
(1) accurately weighing 1g of electronic cigarette tobacco tar, placing the electronic cigarette tobacco tar in a 25mL volumetric flask, performing constant volume with 20% ethanol water solution, and shaking up to obtain a sample solution for later use;
(2) measured with a continuous flow analyzer:
preparing a phenol reagent: weighing 0.10g of MBTH hydrochloride, using 250mL of deionized water to fix the volume, and shaking up;
preparing an ammonium ferric sulfate reagent: weighing 1.00g of ammonium ferric sulfate, using 0.2mol/L hydrochloric acid to fix the volume to 500mL, and shaking up;
preparing a cleaning solution: adding 0.25mL of Brij-35 into 250mL of deionized water, and shaking up;
mixing the sample solution with the phenol reagent by 5 turns of mixing ring, mixing with the ferric ammonium sulfate reagent by 5 turns of mixing ring, feeding the mixed solution into a heating pool, mixing the mixed solution heated to 37 ℃ by 20 turns of mixing ring, and feeding the mixed solution into a detector;
analyzer flow path setup: the sample solution is pumped by an orange/white pump tube at the flow rate of 0.23 mL/min; the flow rate of the phenol reagent is 1.00mL/min by using an ash/ash pump pipe; an orange/white pump pipe is used for the ferric ammonium sulfate reagent, and the flow rate is 0.23 mL/min; the air pipe is a black/black pump pipe, and the flow rate is 0.32 mL/min; the cleaning solution is a blue/blue pump tube, and the flow rate is 1.6 mL/min; detection wavelength: 630 nm; detecting speed: 40 samples/h; sample introduction/cleaning time ratio: 1: 1; baseline correction: opening; and (3) drift correction: opening;
(3) drawing a standard curve: accurately absorbing 2.7mL of 37% formaldehyde solution by using a pipette, diluting with deionized water to a constant volume of 1000mL, and obtaining a standard stock solution; transferring 4mL of standard stock solution by using a pipette, and fixing the volume to 100mL by using deionized water to obtain intermediate solution; respectively transferring 1.5 mL, 3.0 mL, 4.5 mL, 6.0 mL and 7.5mL of intermediate solution by using a pipette, and respectively metering the volume to 100mL by using deionized water to respectively obtain 0.6 mg/L, 1.2 mg/L, 1.8 mg/L, 2.4 mg/L and 3.0mg/L of standard working solution; the standard working curve equation is:y=6.34×10-5x-0.35, correlation coefficient r20.9999; wherein y is the instrumental measurement value of the total content of formaldehyde and acetaldehyde corresponding to the sample solution, and x is the peak height;
(4) and (4) calculating a result:
substituting the instrumental measured value of the total content of formaldehyde and acetaldehyde corresponding to the sample solution into the formula (1) for calculation to obtain the total content of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar to be measured, and taking the average value of two parallel measurements as the final measurement result;
Figure BDA0003010466130000041
in the formula: p is total content (mg/Kg) of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar to be detected, C is instrument measured value (mg/L) of the total content of the formaldehyde and the acetaldehyde corresponding to the sample solution, V is volume (mL) of the extraction solvent, and m is tobacco tar sample mass (g).
Compared with the prior art, the invention has the following advantages:
the invention realizes the accurate determination of the total content of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar by using the continuous flow analyzer for the first time, and the method has the following advantages: the pretreatment is simple: only one-step extraction with ethanol water is needed, and the detection can be carried out on a machine; secondly, the analysis speed is fast: 40 samples can be measured per hour; ③ the anti-interference performance is strong: the color reaction is weakened along with the lengthening of the carbon chain, the total content of formaldehyde and acetaldehyde can be specifically determined, and other aldehydes do not interfere the determination; fourthly, the repeatability and the stability are better: the variation coefficients of 5 samples detected at different time and in different batches are all less than 2%; the accuracy is high: the standard recovery rate range of the total content of the formaldehyde and the acetaldehyde is determined to be 96.50 percent to 106.44 percent; sixthly, the detectable concentration range is wide: the range of measurement is 0-5.4 mg/L; detection limit and quantification limit are as follows: the detection limit of the method is 0.42mg/Kg, and the quantification limit is 1.4 mg/Kg. The method is suitable for detecting the tobacco tar samples of the electronic cigarettes in large batches.
Drawings
FIG. 1 is a schematic view of a flow path setup of a continuous flow analyzer;
FIG. 2 Effect of extraction solvent;
FIG. 3 is a standard working curve map displayed by the instrument software;
FIG. 4 is a standard operating curve automatically drawn by the instrument software.
Detailed Description
The present invention is further described in detail with reference to the drawings and examples, which are not intended to limit the technical scope of the present invention, and all changes and equivalents which are made based on the teachings of the present invention should fall within the protective scope of the present invention.
Example 1
1. Principles of experiment, materials and methods
1.1 principle of the experiment
Aldehyde groups of formaldehyde and acetaldehyde in the electronic cigarette smoke oil react with a phenol reagent to generate oxazine, the oxazine is oxidized by high-iron ions in an acid solution to form a blue-green compound (the reaction is reduced along with the lengthening of a carbon chain, the acrolein hardly generates a color reaction, the measured aldehyde group content is equal to the content of the formaldehyde and the acetaldehyde), the compound has maximum absorption at a wavelength of 630nm, and the total content of the formaldehyde and the acetaldehyde in the electronic cigarette smoke oil can be obtained by monitoring the change of the peak height of an absorption peak and contrasting with a standard working curve through calculation.
1.2 materials and instruments
MBTH hydrochloride (AR, 98.0%, shanghai mclin biochemistry science and technology limited); ammonium ferric sulfate (AR, chemical agents ltd of national drug group); hydrochloric acid (AR, west longridge chemical plant, guangdong, Shantou, Guangdong); 37% formaldehyde (AR, chemical agents ltd of the national drug group); 40% acetaldehyde (AR, chemical agents ltd of the national drug group); ethanol (Shimazu Kagaku, Guangdong, Shantou, Shang, China).
METLER AE200 analytical balance (sensory: 0.0001g, METLER TOLEDO, Switzerland); BRAN LUEBBE AA3 continuous flow analyzer (BRAN LUEBBE, Germany); JA5002 balance (sensory 0.01g, shanghai balance instrument factory); millipore AQUELIX5 water purifier (MERCK Millipore, USA).
1.3 sample treatment and analysis
(1) Sample pretreatment
Weighing 1.0g of electronic cigarette tobacco tar (accurate to 0.1mg) and placing the electronic cigarette tobacco tar in a 25mL volumetric flask, using 20% ethanol water solution for constant volume, shaking up, and using the electronic cigarette tobacco tar as a sample solution for later use;
(2) analysis with continuous flow Analyzer
Preparing a phenol reagent: weighing 0.10g of MBTH hydrochloride, using 250mL of deionized water to fix the volume, and shaking up;
preparing an ammonium ferric sulfate reagent: weighing 1.00g of ammonium ferric sulfate, using 0.2mol/L hydrochloric acid to fix the volume to 500mL, and shaking up;
preparing a cleaning solution: adding 0.25mL of Brij-35 into 250mL of deionized water, and shaking up;
the instrument pipeline diagram is shown in figure 1, a sample solution and a phenol reagent are mixed by 5 circles of mixing rings and then are mixed with an ammonium ferric sulfate reagent by 5 circles of mixing rings, the mixed solution enters a heating pool (the heating temperature is 37 ℃), and the heated mixed solution enters a detector after being mixed and reacted by 20 circles of mixing rings;
the sample solution is pumped by an orange/white pump tube at the flow rate of 0.23 mL/min; the flow rate of the phenol reagent is 1.00mL/min by using an ash/ash pump pipe; an orange/white pump pipe is used for the ferric ammonium sulfate reagent, and the flow rate is 0.23 mL/min; the air pipe is a black/black pump pipe, and the flow rate is 0.32 mL/min; the cleaning solution is a blue/blue pump tube, and the flow rate is 1.6 mL/min; detection wavelength: 630 nm; detecting speed: 40 samples/h; sample introduction/cleaning time ratio: 1: 1; baseline correction: opening; and (3) drift correction: opening;
drawing a standard curve: accurately absorbing 2.7mL of 37% formaldehyde solution by using a pipette, diluting with deionized water to a constant volume of 1000mL, and obtaining a standard stock solution; transferring 4mL of standard stock solution by using a pipette, and fixing the volume to 100mL by using deionized water to obtain intermediate solution; respectively transferring 1.5 mL, 3.0 mL, 4.5 mL, 6.0 mL and 7.5mL of intermediate solution by using a pipette, and respectively metering the volume to 100mL by using deionized water to respectively obtain 0.6 mg/L, 1.2 mg/L, 1.8 mg/L, 2.4 mg/L and 3.0mg/L of standard working solution; the standard working curve equation is: y is 6.34 × 10- 5x-0.35, wherein y is the instrumental measurement of the total content of formaldehyde and acetaldehyde corresponding to the sample solution, x is the peak height, and the correlation coefficient r2=0.9999;
And (4) calculating a result: substituting the instrument measured value of the total content of formaldehyde and acetaldehyde corresponding to the tobacco tar sample solution to be measured into the formula (1) for calculation to obtain the total content of formaldehyde and acetaldehyde in the electronic tobacco tar to be measured, and taking the average value of two parallel measurements as the final measurement result;
Figure BDA0003010466130000061
in the formula: p is total content (mg/Kg) of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar sample to be detected, C is instrument measurement value (mg/L) of the total content of the formaldehyde and the acetaldehyde corresponding to the sample solution, V is volume (mL) of the extraction solvent, and m is tobacco tar sample mass (g).
2. Results and discussion
2.1 Condition optimization
2.1.1 Effect of sample pretreatment extraction solvent
Considering that the main components of the electronic cigarette tobacco tar are a mixture composed of propylene glycol, glycerol, nicotine, various essences and the like, ethanol/water mixed solutions (0%, 10%, 20%, 30%, 40% and 50%) with different volume ratios are selected as pretreatment solvents according to the similar compatibility theorem, and after an electronic cigarette tobacco tar sample 1# is extracted, the electronic cigarette tobacco tar is subjected to on-machine analysis. FIG. 2 shows that: when the volume ratio is 20%, the instrument response value (peak height) corresponding to the target object to be detected is the highest, which indicates that the target object to be detected can be completely extracted under the ethanol aqueous solution with the concentration, and therefore, the extraction solvent is determined to be 20% ethanol aqueous solution.
2.1.2 pipeline preparation of Primary reagents for continuous flow Analyzer
And selecting an appropriate pipeline configuration by comparing the influence of different pipeline configurations of the sample solution, the phenol reagent and the ferric ammonium sulfate reagent on the detection condition. The standard working solution of formaldehyde with concentration of 0.6, 1.2, 1.8, 2.4 and 3.0mg/L is obtained by diluting the 37 percent formaldehyde solution with deionized water step by step. As shown in table 1, the highest formaldehyde content and linear correlation coefficient corresponding to the baseline, peak shape and linearity were examined comprehensively, and the following pipeline configurations were selected: the sample solution and the ammonium ferric sulfate reagent were both pumped through an orange/white pump tube (flow rate of 0.23mL/min) and a phenol reagent through a gray/gray pump tube (flow rate of 1.00 mL/min).
TABLE 1 tubing configuration for the principal reagents of a continuous flow analyzer
Figure BDA0003010466130000071
2.1.3 selection of the number of turns of the chromogenic reaction mixing Ring
The color reaction occurs after the ferric ammonium sulfate reagent is added, so the color reaction time is determined by changing the influence of the total number of turns of the reaction mixing ring after the ferric ammonium sulfate reagent is added on the peak appearance condition. The number of turns of the reaction mixing ring is designed to be 5, 10 and 15, and peak time, peak shape, linear correlation coefficient and the highest formaldehyde content corresponding to linearity are comprehensively considered. The results in table 2 show that when the number of turns of the coil is 5, the reaction time is sufficient, the peak time is the shortest, and the number of turns of the final mixed coil is determined to be 5 in consideration of the detection efficiency.
TABLE 2 selection of number of turns of reactive mixing ring
Figure BDA0003010466130000081
2.2 evaluation of method
2.2.1 Standard Curve and Linear equation
Diluting 37% formaldehyde solution with deionized water step by step to obtain 0.6, 1.2, 1.8, 2.4, 3.0, 3.6, 4.2, 4.8, 5.4 and 6.0mg/L formaldehyde standard working solution in sequence, detecting with the optimal configuration of the instrument determined by 2.1, and finding that the standard solution is linearly related in the concentration range of 0-5.4 mg/L.
However, in consideration of the content concentration range of formaldehyde and acetaldehyde in the electronic cigarette smoke, the formaldehyde standard working solution with the more appropriate concentration range of 0-3mg/L is selected for detection and sample analysis, the spectrum is shown in figure 3, and the standard curve is shown in figure 4. By a linear correlation coefficient r2>0.999 is a criterion, the highest aldehyde group content corresponding to the solution is determined to be 2.994mg/L, and the standard working curve equation obtained in the content range is as follows: y is 6.34 × 10-5x-0.35, correlation coefficient r20.9999, wherein y is the instrumental measurement of the total formaldehyde and acetaldehyde content corresponding to the sample solution,and x is the peak height.
2.2.2 detection and quantitation limits
The blank solution was continuously injected 10 times, and the Standard Deviation (SD) of the measurement results was 0.14, so that the detection limit of the method was 3 SD-0.42 mg/Kg, and the quantification limit was 10 SD-1.4 mg/Kg.
2.2.3 repeatability
Five samples of e-cigarette smoke were tested in parallel by the same experimenter according to the method of the present invention for 3 times in the same time period, and the results are shown in table 3. As can be seen from Table 3, the RSD values of the total content of formaldehyde and acetaldehyde measured by the method are respectively 0.22%, 0.47%, 0.18%, 1.11% and 0.66%, which are all less than 2%, and the repeatability is good.
TABLE 3 repeatability
Figure BDA0003010466130000091
2.2.4 stability
Five samples of e-cigarette smoke were measured by the same operator according to the method of the invention 3 times in different time periods, 2 times in parallel each time, and averaged, the results are shown in table 4. As can be seen from Table 4, the RSD values of the total content of formaldehyde and acetaldehyde measured by the method are respectively 0.21%, 0.48%, 1.14% and 0.45%, which are all less than 2%, and the stability is good.
TABLE 4 stability
Figure BDA0003010466130000092
2.2.5 actual sample analysis and recovery Rate of spiked samples
The low, medium, and high spiked recovery measurements of formaldehyde and acetaldehyde were performed on five samples of e-cigarette smoke using the method of the present invention and resulted in between 96.50% and 106.44% (table 5). The method has good accuracy and reliable detection result.
TABLE 5 sample determination and recovery by spiking
Figure BDA0003010466130000101
2.2.6 anti-interference Performance
Propionaldehyde, acrolein, butyraldehyde and crotonaldehyde which may influence the measurement of the total content of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar sample are selected to carry out an interference experiment, 5.03mg/L of the following substances (propionaldehyde, acrolein, butyraldehyde and crotonaldehyde) are respectively added into a pretreatment extracting solution (the concentration of formaldehyde and acetaldehyde is 0.503mg/L) of a No. 1 sample, and the mixture is mixed and then is put on a computer for analysis. The results show that: the sample No. 1 has a measured value of 0.503mg/L +/-0.05, the interference substances have no influence on the measurement, and the method has better selectivity on aldehyde groups of formaldehyde and acetaldehyde.
3. Conclusion
The method for determining the total content of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar by using the continuous flow analyzer has the advantages of simple and convenient operation, simple pretreatment, high analysis speed, strong anti-interference performance, accurate result, high precision, good repeatability and stability, wide detectable concentration range, low detection limit and quantification limit, and is suitable for detecting a large batch of electronic cigarette tobacco tar samples.

Claims (1)

1. A continuous flow method for measuring the total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar comprises the following steps:
(1) accurately weighing 1g of electronic cigarette tobacco tar, placing the electronic cigarette tobacco tar in a 25mL volumetric flask, performing constant volume with 20% ethanol water solution, and shaking up to obtain a sample solution for later use;
(2) measured with a continuous flow analyzer:
preparing a phenol reagent: weighing 0.10g of MBTH hydrochloride, using 250mL of deionized water to fix the volume, and shaking up;
preparing an ammonium ferric sulfate reagent: weighing 1.00g of ammonium ferric sulfate, using 0.2mol/L hydrochloric acid to fix the volume to 500mL, and shaking up;
preparing a cleaning solution: adding 0.25mL of Brij-35 into 250mL of deionized water, and shaking up;
mixing the sample solution with the phenol reagent by 5 turns of mixing ring, mixing with the ferric ammonium sulfate reagent by 5 turns of mixing ring, feeding the mixed solution into a heating pool, mixing the mixed solution heated to 37 ℃ by 20 turns of mixing ring, and feeding the mixed solution into a detector;
analyzer flow path setup: the sample solution is pumped by an orange/white pump tube at the flow rate of 0.23 mL/min; the flow rate of the phenol reagent is 1.00mL/min by using an ash/ash pump pipe; an orange/white pump pipe is used for the ferric ammonium sulfate reagent, and the flow rate is 0.23 mL/min; the air pipe is a black/black pump pipe, and the flow rate is 0.32 mL/min; the cleaning solution is a blue/blue pump tube, and the flow rate is 1.6 mL/min; detection wavelength: 630 nm; detecting speed: 40 samples/h; sample introduction/cleaning time ratio: 1: 1; baseline correction: opening; and (3) drift correction: opening;
(3) drawing a standard curve: accurately absorbing 2.7mL of 37% formaldehyde solution by using a pipette, diluting with deionized water to a constant volume of 1000mL, and obtaining a standard stock solution; transferring 4mL of standard stock solution by using a pipette, and fixing the volume to 100mL by using deionized water to obtain intermediate solution; respectively transferring 1.5 mL, 3.0 mL, 4.5 mL, 6.0 mL and 7.5mL of intermediate solution by using a pipette, and respectively metering the volume to 100mL by using deionized water to respectively obtain 0.6 mg/L, 1.2 mg/L, 1.8 mg/L, 2.4 mg/L and 3.0mg/L of standard working solution; the standard working curve equation is: y is 6.34 × 10- 5x-0.35, correlation coefficient r20.9999; wherein y is the instrumental measurement value of the total content of formaldehyde and acetaldehyde corresponding to the sample solution, and x is the peak height;
(4) and (4) calculating a result:
substituting the instrumental measured value of the total content of formaldehyde and acetaldehyde corresponding to the sample solution into the formula (1) for calculation to obtain the total content of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar to be measured, and taking the average value of two parallel measurements as the final measurement result;
Figure FDA0003010466120000021
in the formula: p is total content (mg/Kg) of formaldehyde and acetaldehyde in the electronic cigarette tobacco tar to be detected, C is instrument measured value (mg/L) of the total content of the formaldehyde and the acetaldehyde corresponding to the sample solution, V is volume (mL) of the extraction solvent, and m is tobacco tar sample mass (g).
CN202110374014.XA 2021-04-07 2021-04-07 Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar Pending CN113310971A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110374014.XA CN113310971A (en) 2021-04-07 2021-04-07 Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110374014.XA CN113310971A (en) 2021-04-07 2021-04-07 Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar

Publications (1)

Publication Number Publication Date
CN113310971A true CN113310971A (en) 2021-08-27

Family

ID=77371876

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110374014.XA Pending CN113310971A (en) 2021-04-07 2021-04-07 Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar

Country Status (1)

Country Link
CN (1) CN113310971A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103076321A (en) * 2012-11-26 2013-05-01 江苏中烟工业有限责任公司徐州卷烟厂 Method for detecting formaldehyde in water-based adhesive used for cigarette by continuous flow analyzer
CN105954442A (en) * 2016-07-18 2016-09-21 中国烟草总公司郑州烟草研究院 Method for determining formaldehyde in electronic cigarette liquid
CN106198806A (en) * 2016-07-18 2016-12-07 中国烟草总公司郑州烟草研究院 The assay method of acetaldehyde in a kind of tobacco juice for electronic smoke
CN111650189A (en) * 2020-03-13 2020-09-11 云南省烟草质量监督检测站 Method for measuring content of formaldehyde in special slice for cigarette without burning during heating
CN111812047A (en) * 2020-07-01 2020-10-23 云南省烟草质量监督检测站 Method for determining content of total flavonoids in tobacco based on continuous flow analyzer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103076321A (en) * 2012-11-26 2013-05-01 江苏中烟工业有限责任公司徐州卷烟厂 Method for detecting formaldehyde in water-based adhesive used for cigarette by continuous flow analyzer
CN105954442A (en) * 2016-07-18 2016-09-21 中国烟草总公司郑州烟草研究院 Method for determining formaldehyde in electronic cigarette liquid
CN106198806A (en) * 2016-07-18 2016-12-07 中国烟草总公司郑州烟草研究院 The assay method of acetaldehyde in a kind of tobacco juice for electronic smoke
CN111650189A (en) * 2020-03-13 2020-09-11 云南省烟草质量监督检测站 Method for measuring content of formaldehyde in special slice for cigarette without burning during heating
CN111812047A (en) * 2020-07-01 2020-10-23 云南省烟草质量监督检测站 Method for determining content of total flavonoids in tobacco based on continuous flow analyzer

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
侯轶等: "乙醇水溶液提取烟草废弃物的研究", 《烟草化学》, no. 11, pages 56 - 60 *
李广超: "酚试剂分光光度法测定啤酒中的醛类物质", 《广州化工》, vol. 41, no. 19, pages 97 - 98 *
杜茹芸等: "高效液相色谱法测定电子烟雾化液中甲醛、乙醛、 丙烯醛和2, 3 - 丁二酮的含量", 《香料香精化妆品》, no. 1, pages 16 - 20 *
白郁华等: "北京市夏季城近郊区大气醛类含量及分布规律探讨", 《环境科学》, vol. 13, no. 6, pages 75 - 80 *

Similar Documents

Publication Publication Date Title
Španěl et al. Quantification of trace levels of the potential cancer biomarkers formaldehyde, acetaldehyde and propanol in breath by SIFT-MS
CN103163270A (en) Method for detecting eight volatile carbonyl compounds in cigarette filter tip through liquid chromatography-tandem mass spectrometry
CN104142374B (en) A kind of method that adopts directly carbonyl compound content in derive/high-performance liquid chromatogram determination tobacco juice for electronic smoke
CN102353741A (en) Method for measuring contents of four kinds of tobacco-specific nitrosamines in cigarette mainstream smoke
CN105021744A (en) Method for measuring eight carbonyl compounds in electronic cigarette tobacco tar
CN102213714A (en) Detection method for identifying natural taurine and synthesized taurine
CN111505097A (en) Electrochemical method for measuring nicotine content in tobacco and tobacco related products
CN111812047A (en) Method for determining content of total flavonoids in tobacco based on continuous flow analyzer
CN114624303B (en) Electrochemical method for rapidly and quantitatively determining nicotine in electronic cigarette
CN111279190B (en) Method for detecting aldehydes and ketones using thin layer chromatography
CN113310971A (en) Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar
CN107703222B (en) Method for determining trace organic amine in atmospheric particulates
CN102353739A (en) Rapid detection method of nicotine in tobacco
CN111257452B (en) Method for detecting addition of synthetic acetic acid into Zhenjiang aromatic vinegar
CN113310972A (en) Method for measuring acetaldehyde content in tobacco tar of electronic cigarette
CN109975444A (en) The measuring method of Alkaloid and nitrosamine in a kind of buccal cigarette
CN106018635B (en) The method and detection method of pre-treatment are carried out to tobacco or tobacco product
CN109765215B (en) Raman spectrum quantitative analysis method for organic matters in titanium tetrachloride
CN113310913A (en) Intermittent chemical method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar
CN101498670B (en) Method for measuring nitrogen oxide in cigarette side-stream smoke
CN106093235A (en) A kind of for measuring moisture and the extract of nicotine content and using method thereof in cigarette mainstream flue gas
CN108693286B (en) Method for detecting genotoxic impurity diisopropyl sulfate in medicine
CN111380817A (en) Method for measuring total sulfur dioxide in tobacco or tobacco products by continuous flow method
CN103091438B (en) Method for measuring benzo [a] pyrene content in cigarette filter
CN114252418A (en) Method for detecting acetaldehyde in wine sample by using fluorescent probe

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination