Method for measuring eight carbonyl compounds in electronic cigarette tobacco tar

A carbonyl compound and e-cigarette liquid technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of affecting the measurement results, restricting applications, and large differences in ratios, and achieves good repeatability, high sensitivity, and fewer impurity peaks Effect

Inactive Publication Date: 2015-11-04
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Application Information

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Problems solved by technology

Since the e-cigarette liquid matrix is ​​mainly composed of glycerin and propylene glycol, and the ratio of the two in the matrix is ​​very different, and glycerol and acetonitrile are immiscible, when using this method to process samples, some samples will appear delamination phenomenon, affecting The results of the determination limit the application of the method

Method used

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  • Method for measuring eight carbonyl compounds in electronic cigarette tobacco tar
  • Method for measuring eight carbonyl compounds in electronic cigarette tobacco tar
  • Method for measuring eight carbonyl compounds in electronic cigarette tobacco tar

Examples

Experimental program
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Effect test

example 1

[0025] Standard working solutions with different concentrations were injected into HPLC, and the limit of detection (LOD) was calculated with a 3-fold signal-to-noise ratio (S / N = 3), and the detection limit was between 0.029 μg / g and 0.076 μg / g. The spiked recovery experiment was carried out at three concentration levels of low, medium and high, and the experiments were carried out in parallel for 5 times, and the results were averaged (see Table 2). The results showed that the recoveries of eight carbonyl compounds ranged from 91.1% to 102.3%, and the average relative standard deviation (RSD) was less than 6.0%.

[0026] Table 2 Recovery and repeatability of 8 carbonyl compounds (n=5)

[0027] serial number Compound name LOD(μg / g) Recovery rate(%) RSD (%) 1 formaldehyde 0.029 97.5 3.8 2 Acetaldehyde 0.037 91.1 4.5 3 acetone 0.048 100.2 4.3 4 acrolein 0.044 90.3 5.1 5 ...

example 2

[0029] Weigh 0.5 g of e-cigarette liquid, add DNPH derivatization reagent, dilute to 5 mL, shake well, place at room temperature for 30-150 min for derivatization reaction, pass the reaction solution through a 0.45 μm organic phase filter membrane; pipette 0.5 mL for reaction solution, and added 0.5 mL of Tris base, shaken, into the HPLC analysis. The measurement was repeated 5 times, and the relative standard deviation was calculated to obtain the precision of the method.

[0030] Table 3 Method precision

[0031]

[0032] Note: N.D. is not detected.

example 3

[0034] A commercially available mint-flavored e-cigarette liquid was pretreated according to the method described in Example 2 and tested by HPLC. The contents of the eight carbonyl compounds in the e-cigarette liquid sample were: formaldehyde 12.03 μg / g, acetaldehyde 0.03 μg / g, acetone 0.39 μg / g, acrolein 0.78 μg / g, propionaldehyde, crotonaldehyde, 2-butanone and butyraldehyde were not detected.

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Abstract

The invention belongs to the field of analysis of harmful ingredients of an electronic cigarette and particularly relates to a method for measuring eight carbonyl compounds in electronic cigarette tobacco tar. The method is characterized in that a DNPH (dinitrophenylhydrazine) solution prepared from diluted hydrochloric acid and the carbonyl compounds in the electronic cigarette tobacco tar have a derivatization reaction, pH (potential of hydrogen) of the reaction solution is adjusted with Tris (trihydroxymethyl aminomethane) base, stability of a reaction product is kept, and the eight carbonyl compounds in the electronic cigarette tobacco tar are analyzed and measured with HPLC (high performance liquid chromatography). The method has the advantages as follows: the sample pretreatment process is simple and rapid; a DNPH derivatization reagent and the Tris base are prepared with deionized water, no organic reagent is used in the pretreatment process, and the method is green and environment-friendly. The method is accurate in measurement, high in sensitivity and good in repeatability and can provide a technical support for product quality control of the electronic cigarette tobacco tar.

Description

Technical field [0001] The invention involves the analysis and measurement method of eight types of cymbal compounds in the electronic smoke liquid, and specifically refers to the reaction of the 2,4-diitol (DNPH) derivative of 2,4-diitol (DNPH) prepared by dilute hydrochloric acid solution.Then add trimader aminitoral methane hydramal solution (TRIS) to regulate the pH of the reaction solution to prevent the aggregation of the reaction product, and then use high-efficiency liquid chromatography (HPLC-DAD) analysis to determine 8 types of cymbal compounds in the electronic smoke liquid. Background technique [0002] In recent years, with the continuous increase in global smoke control, the sales of traditional cigarettes in some developed countries have declined, and the global sales of electronic cigarettes have grown rapidly.Electronic cigarettes, also known as electronic atomization cigarettes, are an electronic device that transmits Nigerin to the respiratory system through e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 潘立宁赵乐刘绍锋余晶晶樊美娟蔡君兰刘克建陈黎于永杰孙培健刘惠民
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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