CN105954442A - Method for determining formaldehyde in electronic cigarette liquid - Google Patents
Method for determining formaldehyde in electronic cigarette liquid Download PDFInfo
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- CN105954442A CN105954442A CN201610563461.9A CN201610563461A CN105954442A CN 105954442 A CN105954442 A CN 105954442A CN 201610563461 A CN201610563461 A CN 201610563461A CN 105954442 A CN105954442 A CN 105954442A
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- formaldehyde
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- tobacco juice
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
Abstract
The invention relates to a rapid analysis method for determining formaldehyde in electronic cigarette liquid. The method comprises the following steps that firstly, a dispersant is added to an electronic cigarette liquid sample, then a DNPH derivatization reagent and an acid solution are added to perform derivatization reaction, an alkaline reagent and an internal standard substance are added, and finally the formaldehyde content in the electronic cigarette liquid is determined through LC-MS/MS analysis. The method is high in sensitivity, strong in anti-interference performance and good in repeatability, the pretreatment process is simple and rapid, and the method is suitable for detection of electronic cigarette liquid samples on a large scale.
Description
Technical field
The present invention relates to the fast analysis determination method of formaldehyde in a kind of tobacco juice for electronic smoke, belong to Analytical Methods of Trace neck
Territory.
Background technology
Formaldehyde, has another name called formaldehyde, under room temperature be a kind of colourless, there is the gas of intense stimulus.Formaldehyde is moderate toxicity thing
Matter, LD50800 mg/kg(rat orals)；60~120 mg/m3Bronchus and pulmonary is i.e. occurred seriously to damage after sucking 5 ~ 10 min
Evil.Per os lethal dose is about 10 ~ 20 mL.Acute formaldehyde poisoning is mainly based on eye, respiratory system and central nervous system damage
Systemic disease.Long Term Contact low concentration formaldehyde steam, can have the symptom such as headache, weakness to occur.Numerous studies show
Formaldehyde has mutagenicity and carcinogenecity, and international cancer research institution (IARC) is classified as 1 class human carcinogen.
In recent years, along with whole world Tobacco Control dynamics continues to increase, the sales volume in some developed country's traditional cigarette occurs in that one
Fixed downward trend, and electronic cigarette is in the global sales gesture in quickly growth.Electronic cigarette, also known as electrospray Medicated cigarette, is a kind of logical
Cross electronics heater means and transmit the electronic installation of nicotine to respiratory system.It is molten that tobacco juice for electronic smoke refers to produce gas for electronic cigarette
Glue, the liquid aspirated for consumer or gel, great majority are by propylene glycol, glycerol, nicotine and the various perfume (or spice) improving mouthfeel
The mixture of the compositions such as essence.At present, in cigarette smoke and smoking material, the assay method document report of formaldehyde is more, mainly has
Gas chromatography, liquid chromatography and liquid chromatography tandem mass spectrometry etc..Electronic cigarette, as a kind of novel tobacco goods, is grasped
The contents level of formaldehyde in tobacco juice for electronic smoke, is favorably improved electronic cigarette product safety quality monitoring.Therefore, a kind of energy is set up
The most quickly measuring the assay method of formaldehyde in tobacco juice for electronic smoke, tool is of great significance.
[8 kinds of volatile carbonyl compounds [J], the Agriculture of Anhui in high effective liquid chromatography for measuring tobacco juice for electronic smoke such as Chen Gang
Science, 2014,42 (31): 11072] use the DNPH solution of acetontrile to occur anti-with carbonyl compound in tobacco juice for electronic smoke
Should, then extract solution constant volume with pyridine/acetonitrile (V:V=1:50), then use HPLC can detect tobacco juice for electronic smoke and include
Formaldehyde is at 8 kinds of interior volatile carbonyl compounds.Owing to tobacco juice for electronic smoke substrate is mainly made up of glycerol, propylene glycol, and substrate
Both in, ratio difference is very big, and glycerol and both acetonitriles are immiscible, when causing using the method to process sample, and part sample
There is lamination in product, affect measurement result, limit the application of the method.[8 kinds of carbonyl compounds in a kind of tobacco juice for electronic smoke
Assay method] (publication number CN105021744A) use carbonyl in DNPH solution and the tobacco juice for electronic smoke of aqueous hydrochloric acid solution preparation
Compound reacts, and uses 8 kinds of carbonyl compounds of liquid chromatogram measuring.The method reaction system is homogeneous, it is to avoid layering
The generation of phenomenon.From two document testing results, in tobacco juice for electronic smoke, content of formaldehyde is μ g/g level, and content is relatively low.Further,
Owing to tobacco juice for electronic smoke brand specification is of a great variety, different taste tobacco juice for electronic smoke additive differs greatly, and causes electronic cigarette
Liquid-based matter is more complicated, and different tobacco juice for electronic smoke sample substrate is widely different.Low concentration sample in complex matrices is carried out
Quantitative analysis, Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) has obvious advantage: LC-MS/MS and uses multiple-reaction monitoring pattern
(MRM), selectivity is good, highly sensitive, can effectively eliminate impurity interference, even if chromatograph fails to be kept completely separate material, it is also possible to
Identify, the qualitative and quantitative detection of trace materials during therefore LC-MS/MS is commonly used for complex matrices sample.
Summary of the invention
The purpose of the present invention is based on above-mentioned prior art situation and establishes a kind of employing LC-MS/MS mensuration electronic cigarette
The method of formaldehyde in tobacco juice, the method pre-treatment is simple, can quickly, content of formaldehyde in Accurate Determining tobacco juice for electronic smoke, and be suitable for
In various ratio glycerin/propylene glycol tobacco juice for electronic smoke matrix sample.
It is an object of the invention to be achieved through the following technical solutions:
The assay method of formaldehyde in a kind of tobacco juice for electronic smoke, including following sample pre-treatments: accurately weigh tobacco juice for electronic smoke sample,
Adding dispersant deionized water, add DNPH derivatization reagent and acid solution, room temperature placement certain time performs the derivatization instead
Should, after reaction terminates, add alkaline reagent and internal standard substance, after constant volume, cross organic facies filter membrane, use LC-MS/MS to detect electronics
Content of formaldehyde in cigarette tobacco juice sample, specifically comprises the following steps that
(1) sample pre-treatments: accurately weigh tobacco juice for electronic smoke sample in 10 mL volumetric flasks, adds example weight 3～15 times
Water, is subsequently adding every gram of sample 2～15 mL DNPH derivatization reagent, adds 50～500 L HClO4Aqueous solution, shakes up, room
Temperature is placed 30～150 min and is performed the derivatization reaction, and reaction is initially charged 50～500 L pyridines after terminating, is subsequently adding 100 L
Internal standard working solution, crosses organic facies filter membrane after acetonitrile constant volume, enter LC-MS/MS and analyze；
(2) standard solution preparation:
Standard reserving solution (100 g/mL): weigh in 10 mg formaldehyde 2,4 dinitrophenylhydrazone standard substance to 100 mL volumetric flasks,
It is settled to scale by dilution in acetonitrile.Stored protected from light under the conditions of-18 DEG C, 6 months effect duration.
Internal standard storing solution (1000 g/mL): weigh the internal standard substance of 10 mg in 10 mL brown volumetric flasks is dilute with acetonitrile
Release and be settled to scale.Stored protected from light under the conditions of-18 DEG C, 6 months effect duration.
Internal standard working solution (20 g/mL): pipette in internal standard storing solution 2 mL to 100 mL volumetric flask, fixed by dilution in acetonitrile
Hold to scale.Stored protected from light under the conditions of-18 DEG C, 6 months effect duration.
Standard working solution: pipette respectively standard reserving solution 2 μ L, 5 μ L, 10 μ L, 20 μ L, 50 μ L, 100 μ L,
In 200 μ L and 500 μ L to 8 10 mL brown volumetric flasks, each volumetric flask moves into 100 μ L internal standard working solutions, uses acetonitrile
Dilution is settled to scale.(3) LC-MS/MS analyzes:
A, high-efficient liquid phase chromatogram condition:
Chromatographic column: anti-phase C18 liquid-phase chromatographic column；Column temperature: 20～30 DEG C；Sample size: 1～10 μ L；Mobile phase A: water；Flowing phase
B: acetonitrile；Type of elution: isocratic elution；Flow velocity: 0.1～0.5 mL/min；Analysis time: 15 min；
B, Mass Spectrometry Conditions:
Ion source: electron spray ionisation source (ESI)；Scan mode: anion scans；Detection mode: multiple-reaction monitoring pattern
(MRM)；Electron spray voltage :-3000～-5000 V；Ion source temperature: 300～500 DEG C.Object monitoring ion pair see table:
(4) measurement result and calculating
First standard working solution is detected under the conditions of above-mentioned LC-MS/MS, by object and internal standard quota ion to peak
Area ratio and concentration of formaldehyde carry out regression analysis, obtain formaldehyde standard working curve and regression equation；
Secondly sample solution is detected under above-mentioned the same terms, obtain determinand and internal standard quota ion to peak area ratio
Value, is substituted in regression equation, obtains concentration of formaldehyde in sample solution, and calculate content of formaldehyde in sample.
In the present invention, DNPH derivatization reagent is individually prepared with acid solution；Preparation DNPH derivatization reagent uses
Solvent is acetonitrile；The acid that preparation acid solution uses is HClO4, diluent is deionized water.
Described internal standard substance isd 3 Formaldehyde 2,4 dinitrophenylhydrazone ord 3 Acetaldehyde 2,4 dinitrophenylhydrazone.
It is an advantage of the current invention that:
The present invention measures the method for formaldehyde in tobacco juice for electronic smoke, adds dispersant deionized water in tobacco juice for electronic smoke sample,
Purpose is to make reaction system homogeneous, does not haves lamination, and the method is applicable to various ratio glycerin/propylene glycol electronic cigarette
Liquid-based quality sample；DNPH derivatization reagent and acid solution, the two is individually prepared, and can effectively prevent DNPH derivatization reagent from existing
React with aldoketones material in air under acid condition；Preparation DNPH derivatization reagent uses acetonitrile, owing to DNPH is in second
Favorable solubility in nitrile, and compared to alcohols solvent, acetonitrile will not introduce aldoketones impurity；The acid solution that this method uses is
HClO4Aqueous solution, relative to other acid such as HCl, HClO4Reaction efficiency is higher, and after employing deionized water dilution, can prevent office
Portion's acetonitrile meets strong acid hydrolysis；This method adds alkaline reagent pyridine after derivative reaction terminates, owing to pyridine is at acetonitrile/water body
Having good dissolubility in system, and product can be prevented to be polymerized, keep product stability, measurement result is more accurate
Really；Additionally, the method uses LC-MS/MS to be measured formaldehyde in tobacco juice for electronic smoke, method is highly sensitive, strong interference immunity,
Reproducible, and pretreatment process is simple, quick, is suitable for the detection of high-volume tobacco juice for electronic smoke sample.
Accompanying drawing explanation
Fig. 1 is that the standard working solution MRM of the inventive method schemes (target composite diagram in adding two kinds respectively),
In figure: a. formaldehyde hydrazone a'.d 3Formaldehyde hydrazone b'.d 3Acetaldehyde hydrazone.
Specific embodiments
The present invention is described further below in conjunction with instantiation, but is not limiting as the present invention.
Example 1
Formaldehyde 2,4 dinitrophenylhydrazone standard solution enters LC-MS/MS and analyzes.By object and internal standard quota ion to peak area
Ratio and concentration of formaldehyde carry out regression analysis, obtain formaldehyde standard working curve and regression equation, with 3 times of signal to noise ratios (S/N=
3) calculating detection limit (LOD), concrete testing result is shown in Table 2:
The testing result of table 2 formaldehyde standard working solution
| Compound | Linear equation | Correlation coefficient | Detection limit/(ng/g) | Quantitative limit/(ng/g) |
| Formaldehyde | y=0.056x+0.069 | 0.9991 | 28 | 93 |
Example 2
Carrying out recovery of standard addition experiment at basic, normal, high 3 concentration levels, each mark-on level is repeated 6 times, according to measured quantity and
Add each pitch-based sphere of Scalar operation the response rate and precision, concrete outcome see table:
The table 3 method response rate and repeatability
Example 3
Weigh certain tobacco juice for electronic smoke sample 0.2 g, be separately added into 0.6～3.0 mL deionized waters, 0.4～3.0 mL DNPH spread out
Biochemical reagents and 50～500 L HClO4Aqueous solution, shakes up, and room temperature is placed 30～150 min and performed the derivatization reaction, instead
50～500 L pyridines should be added after terminating, add 100 L internal standard working solutions, and be settled to 10 mL with acetonitrile, shake up, mistake
0.22 m organic facies filter membrane, enters LC-MS/MS and analyzes.
Object and internal standard quota ion are substituted into regression equation to peak area ratio, calculates content of formaldehyde in sample
It is 0.47 g/g.
Claims (5)
1. the assay method of formaldehyde in a tobacco juice for electronic smoke, it is characterised in that: include following sample pre-treatments: accurately weigh electricity
Sub-cigarette tobacco juice sample, adds dispersant, adds DNPH derivatization reagent and acid solution, and room temperature placement certain time derives
Change reaction, after reaction terminates, add alkaline reagent and internal standard substance, after constant volume, cross organic facies filter membrane, use LC-MS/MS detection
Content of formaldehyde in tobacco juice for electronic smoke sample, specifically comprises the following steps that
(1) sample pre-treatments: accurately weigh tobacco juice for electronic smoke sample in 10 mL volumetric flasks, adds example weight 3～15 times points
Powder, is subsequently adding every gram of sample 2～15 mL DNPH derivatization reagent, adds 50～500 L HClO4Aqueous solution, shakes up,
Room temperature is placed 30～150 min and is performed the derivatization reaction, and reaction is initially charged 50～500 L pyridines after terminating, is subsequently adding 100
L internal standard working solution, crosses organic facies filter membrane after acetonitrile constant volume, enter LC-MS/MS and analyze；
(2) standard solution preparation:
Standard reserving solution: weigh in 10 mg formaldehyde 2,4 dinitrophenylhydrazone standard substance to 100 mL volumetric flasks, use dilution in acetonitrile
It is settled to scale；
Internal standard storing solution: weigh the internal standard substance of 10 mg in 10 mL brown volumetric flasks, be settled to scale by dilution in acetonitrile；
Internal standard working solution: pipette in internal standard storing solution 2 mL to 100 mL volumetric flask, be settled to scale by dilution in acetonitrile；
Standard working solution: pipette standard reserving solution 2 μ L, 5 μ L, 10 μ L, 20 μ L, 50 μ L, 100 μ L, 200 μ L respectively
With in 500 μ L to 8 10 mL brown volumetric flasks, each volumetric flask moves into 100 μ L internal standard working solutions, fixed by dilution in acetonitrile
Hold to scale；
(3) LC-MS/MS analyzes:
A, high-efficient liquid phase chromatogram condition:
Chromatographic column: anti-phase C18 liquid-phase chromatographic column；Column temperature: 20～30 DEG C；Sample size: 1～10 μ L；Mobile phase A: water；Flowing phase
B: acetonitrile；Type of elution: isocratic elution；Flow velocity: 0.1～0.5 mL/min；Analysis time: 15 min；
B, Mass Spectrometry Conditions:
Ion source: electron spray ionisation source (ESI)；Scan mode: anion scans；Detection mode: multiple-reaction monitoring pattern
(MRM)；Electron spray voltage :-3000～-5000 V；Ion source temperature: 300～500 DEG C；
(4) measurement result and calculating
First standard working solution is detected under the conditions of above-mentioned LC-MS/MS, by object and internal standard quota ion to peak
Area ratio and concentration of formaldehyde carry out regression analysis, obtain formaldehyde standard working curve and regression equation；
Secondly sample solution is detected under above-mentioned the same terms, obtain determinand and internal standard quota ion to peak area ratio
Value, is substituted in regression equation, obtains concentration of formaldehyde in sample solution, and calculate content of formaldehyde in sample.
The assay method of formaldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: the dispersant of addition
For deionized water.
The assay method of formaldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: DNPH derivatization tries
Agent is individually prepared with acid solution；The solvent that preparation DNPH derivatization reagent uses is acetonitrile；The acid that preparation acid solution uses
For HClO4, diluent is deionized water.
The assay method of formaldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: described internal standard substance isd 3 Formaldehyde 2,4 dinitrophenylhydrazone ord 3 Acetaldehyde 2,4 dinitrophenylhydrazone.
The assay method of formaldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: matter in step (3)
Object monitoring ion pair in spectral condition see table:
。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107255688A (en) * | 2017-05-04 | 2017-10-17 | 东华大学 | The detection method of aldoketones organic volatile in a kind of in-car textile |
| CN108333277A (en) * | 2018-05-11 | 2018-07-27 | 东莞市中鼎检测技术有限公司 | The detection method of acetaldehyde in a kind of dyestuff |
| CN108426969A (en) * | 2018-06-15 | 2018-08-21 | 广东联捷生物科技有限公司 | A kind of analysis method of water soluble aldehyde substance |
| CN111413393A (en) * | 2019-12-20 | 2020-07-14 | 杭州师范大学 | Method for rapidly detecting formaldehyde content in food by high-throughput reaction paper spray mass spectrometry |
| CN112505227A (en) * | 2020-12-29 | 2021-03-16 | 广西中烟工业有限责任公司 | Analysis method for simultaneously determining 11 components in electronic cigarette liquid |
| CN113310971A (en) * | 2021-04-07 | 2021-08-27 | 云南省烟草质量监督检测站 | Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar |
| CN113310913A (en) * | 2021-04-07 | 2021-08-27 | 云南省烟草质量监督检测站 | Intermittent chemical method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar |
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| CN104267135A (en) * | 2014-10-10 | 2015-01-07 | 安徽中烟工业有限责任公司 | Method for measuring carbonyl compound in electronic cigarette liquid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107255688A (en) * | 2017-05-04 | 2017-10-17 | 东华大学 | The detection method of aldoketones organic volatile in a kind of in-car textile |
| CN108333277A (en) * | 2018-05-11 | 2018-07-27 | 东莞市中鼎检测技术有限公司 | The detection method of acetaldehyde in a kind of dyestuff |
| CN108426969A (en) * | 2018-06-15 | 2018-08-21 | 广东联捷生物科技有限公司 | A kind of analysis method of water soluble aldehyde substance |
| CN111413393A (en) * | 2019-12-20 | 2020-07-14 | 杭州师范大学 | Method for rapidly detecting formaldehyde content in food by high-throughput reaction paper spray mass spectrometry |
| CN112505227A (en) * | 2020-12-29 | 2021-03-16 | 广西中烟工业有限责任公司 | Analysis method for simultaneously determining 11 components in electronic cigarette liquid |
| CN113310971A (en) * | 2021-04-07 | 2021-08-27 | 云南省烟草质量监督检测站 | Continuous flow method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar |
| CN113310913A (en) * | 2021-04-07 | 2021-08-27 | 云南省烟草质量监督检测站 | Intermittent chemical method for measuring total content of formaldehyde and acetaldehyde in electronic cigarette tobacco tar |
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