CN105954443A - Method for determining crotonaldehyde in electronic cigarette liquid - Google Patents

Method for determining crotonaldehyde in electronic cigarette liquid Download PDF

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Publication number
CN105954443A
CN105954443A CN201610563618.8A CN201610563618A CN105954443A CN 105954443 A CN105954443 A CN 105954443A CN 201610563618 A CN201610563618 A CN 201610563618A CN 105954443 A CN105954443 A CN 105954443A
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solution
sample
internal standard
tobacco juice
electronic smoke
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潘立宁
赵乐
樊美娟
秦亚琼
郭军伟
陈黎
刘绍锋
王洪波
贾云祯
刘惠民
孟庆华
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Zhengzhou Tobacco Research Institute of CNTC
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Zhengzhou Tobacco Research Institute of CNTC
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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
    • 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

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention relates to a rapid analysis method for determining crotonaldehyde 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 crotonaldehyde 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

The assay method of crotonic aldehyde in a kind of tobacco juice for electronic smoke
Technical field
The present invention relates to the fast analysis determination method of crotonic aldehyde in a kind of tobacco juice for electronic smoke, belong to Analytical Methods of Trace neck Territory.
Background technology
Crotonic aldehyde i.e. crotonaldehyde, for water white transparency to faint yellow flammable liquid, has asphyxiating penetrating odor, belongs to poisoning Class material, LD50240 mg/kg(its mouse oral)；Minimal toxic concentration (stimulates): people sucks 12 mg/m3×10 min.To eye Conjunctiva and upper respiratory tract mucosa have intense stimulus effect.Long Term Contact causes chronic rhinitis, nervous system disorder.At present, Crotonic aldehyde is one of China's tobacco business Medicated cigarette hazardness index characteristic index.
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 crotonic aldehyde is more, mainly There are gas chromatography, liquid chromatography and liquid chromatography tandem mass spectrometry etc..Electronic cigarette is as a kind of novel tobacco goods, the palm Hold the contents level of crotonic aldehyde in tobacco juice for electronic smoke, be favorably improved electronic cigarette product safety quality monitoring.Therefore, one is set up Planting and can the most quickly measure the assay method of crotonic aldehyde 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 Crotonic aldehyde 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 base In matter, the two ratio difference is very big, and glycerol and both acetonitriles are immiscible, when causing using the method to process sample, and part There is lamination in sample, affects measurement result, limits the application of the method.[8 kinds of carbonyl compounds in a kind of tobacco juice for electronic smoke The assay method of thing] (publication number CN105021744A) use carbonyl in DNPH solution and the tobacco juice for electronic smoke of aqueous hydrochloric acid solution preparation Based compound reacts, and uses 8 kinds of carbonyl compounds of liquid chromatogram measuring.The method reaction system is homogeneous, it is to avoid point The generation of layer phenomenon.From two document testing results, in tobacco juice for electronic smoke, Fructus Crotonis aldehyde 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 electronics Cigarette tobacco juice substrate is more complicated, and different tobacco juice for electronic smoke sample substrate is widely different.For low concentration sample in complex matrices Carrying 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 by material, also Can 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 crotonic aldehyde in tobacco juice, the method pre-treatment is simple, can quickly, Fructus Crotonis aldehyde in Accurate Determining tobacco juice for electronic smoke, and It is applicable to 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 crotonic aldehyde in a kind of tobacco juice for electronic smoke, including following sample pre-treatments: accurately weigh tobacco juice for electronic smoke sample Product, add dispersant deionized water, add DNPH derivatization reagent and acid solution, and room temperature placement certain time performs the derivatization Reaction, after reaction terminates, adds alkaline reagent and internal standard substance, crosses organic facies filter membrane after constant volume, uses LC-MS/MS detection electricity Fructus Crotonis aldehyde in sub-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 10 mg crotonic aldehyde 2,4 dinitrophenylhydrazone standards Product, in 100 mL volumetric flasks, are 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 crotonic aldehyde concentration carry out regression analysis, obtain crotonic aldehyde 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 Fructus Crotonis aldehyde concentration in sample solution, and calculate Fructus Crotonis aldehyde 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 crotonic aldehyde in tobacco juice for electronic smoke, adds dispersant deionization in tobacco juice for electronic smoke sample Water, it is therefore an objective to make reaction system homogeneous, does not haves lamination, and the method is applicable to various ratio glycerin/propylene glycol electronics Cigarette tobacco juice matrix sample；DNPH derivatization reagent and acid solution, the two is individually prepared, and can effectively prevent DNPH derivatization from trying Agent reacts with aldoketones material in air in acid condition；Preparation DNPH derivatization reagent uses acetonitrile, due to DNPH Favorable solubility in acetonitrile, and compared to alcohols solvent, acetonitrile will not introduce aldoketones impurity；The acidity that this method uses is molten Liquid is HClO4Aqueous solution, relative to other acid such as HCl, HClO4Reaction efficiency is higher, and after employing deionized water dilution, can prevent Only local acetonitrile meets strong acid hydrolysis；This method adds alkaline reagent pyridine after derivative reaction terminates, due to pyridine acetonitrile/ Having good dissolubility in aqueous systems, and product can be prevented to be polymerized, keep product stability, measurement result is more Add accurately；Additionally, the method uses LC-MS/MS to be measured crotonic aldehyde in tobacco juice for electronic smoke, method is highly sensitive, anti-dry Immunity is strong, 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. crotonic aldehyde 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
Crotonic aldehyde 2,4 dinitrophenylhydrazone standard solution enters LC-MS/MS and analyzes.By object and internal standard quota ion to face, peak Long-pending ratio carries out regression analysis with crotonic aldehyde concentration, obtains crotonic aldehyde standard working curve and regression equation, with 3 times of signal to noise ratios (S/N=3) calculate detection limit (LOD), and concrete testing result is shown in Table 2:
The testing result of table 2 crotonic aldehyde standard working solution
Compound Linear equation Correlation coefficient Detection limit/(ng/g) Quantitative limit/(ng/g)
Crotonic aldehyde y=0.039x+0.081 0.9999 27 90
Example 2
Carrying out recovery of standard addition experiment at basic, normal, high 3 concentration levels, each mark-on level is repeated 5 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 crotonic aldehyde in sample and contain Amount is 0.13 μ g/g.

Claims (5)

1. the assay method of crotonic aldehyde in a tobacco juice for electronic smoke, it is characterised in that: include following sample pre-treatments: accurately weigh Tobacco juice for electronic smoke sample, adds dispersant, adds DNPH derivatization reagent and acid solution, and room temperature is placed certain time and spread out Biochemical reaction, after reaction terminates, adds alkaline reagent and internal standard substance, crosses organic facies filter membrane after constant volume, uses LC-MS/MS inspection Survey Fructus Crotonis aldehyde in tobacco juice for electronic smoke sample, specifically comprise 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 crotonic aldehyde 2,4 dinitrophenylhydrazone standard substance to 100 mL volumetric flasks is dilute with acetonitrile Release and be 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 crotonic aldehyde concentration carry out regression analysis, obtain crotonic aldehyde 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 Fructus Crotonis aldehyde concentration in sample solution, and calculate Fructus Crotonis aldehyde in sample.
The assay method of crotonic aldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: the dispersion of addition Agent is deionized water.
The assay method of crotonic aldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: DNPH derivatization Reagent is individually prepared with acid solution；The solvent that preparation DNPH derivatization reagent uses is acetonitrile；Preparation acid solution uses Acid is HClO4, diluent is deionized water.
The assay method of crotonic aldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: described internal standard substance Ford 3 Formaldehyde 2,4 dinitrophenylhydrazone ord 3 Acetaldehyde 2,4 dinitrophenylhydrazone.
The assay method of crotonic aldehyde in a kind of tobacco juice for electronic smoke, it is characterised in that: in step (3) Object monitoring ion pair in Mass Spectrometry Conditions see table:
。
CN201610563618.8A 2016-07-18 2016-07-18 Method for determining crotonaldehyde in electronic cigarette liquid Pending CN105954443A (en)

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CN115368269A (en) * 2022-07-07 2022-11-22 国家烟草质量监督检验中心 Preparation method of crotonaldehyde-2, 4-dinitrophenylhydrazone standard substance and standard substance prepared by same
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Application publication date: 20160921