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Method for determining content of free nicotine and nicotine salt in electronic cigarette liquid and smoke aerosol

A technology of electronic cigarette liquid and nicotine salt, which is applied in the direction of measuring devices, material separation, instruments, etc., can solve problems such as inability to distinguish nicotine and nornicotine, not suitable for determining electronic cigarette liquid, and different maximum absorption wavelengths

Inactive Publication Date: 2020-06-23
CHINA TOBACCO HUNAN INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the pretreatment of nicotine determination by ultraviolet spectrophotometry is more time-consuming, which is not conducive to rapid analysis.
The gravimetric method of silicotungstic acid can get more accurate results, but the disadvantage is that the analysis time is too long (one analysis cycle is 24-48 h); Sum;
[0012] The determination of free nicotine by liquid chromatography, due to the easy exchange of protonated nicotine and silicon hydroxyl, the nicotine peak is easy to tail
The polarity of nicotine will increase after salt formation, and there may be differences in the peaks on the liquid chromatography column, and the nicotine salts formed by different acids may have different maximum absorption wavelengths due to the different groups of different acids. will be different, so liquid chromatography is not suitable for the determination of nicotine and nicotine salts in e-liquid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take 0.43g of free nicotine and dilute it to 10.0190g with an aerosol containing propylene glycol and glycerol. The theoretical value for free nicotine is 41.15 mg / g. Take 100 μL of the above e-cigarette liquid and dilute it to 10 mL with an isopropanol solution containing heptadecane, combine the internal standard method and the external standard method, and use a gas chromatograph equipped with a hydrogen flame detector to determine the nicotine content in the e-cigarette liquid. The chromatographic column is a strong polar elastic quartz capillary column, the column length is 30m, the inner diameter is 0.32mm, and the film thickness is 1.8μm. Such as DB-ALC1. Temperature program: the initial temperature was 100 °C (hold for 1 min), increased to 130 °C at a rate of 15 °C / min, increased to 220 °C at a rate of 40 °C / min, and held for 10 min. The content of nicotine in the e-cigarette liquid was determined to be 41.68 mg / g. The measured value is consistent with the th...

Embodiment 2

[0028] Take 0.4274g free nicotine and 0.2148g nicotine tartrate diluted to 10.1000g with an aerosol containing propylene glycol and glycerol. The theoretical value of free nicotine is 39.77 mg / g, and the total amount of nicotine is 46.89 mg / g. Take 100 μL of the above e-cigarette liquid and dilute it to 10 mL with an isopropanol solution containing heptadecane, and combine the internal standard method and the external standard method to determine the total amount of nicotine in the e-cigarette liquid to be 47.18 mg / g. Consistent with the theoretical value of total nicotine.

[0029]The e-liquid was diluted with distilled water with pH=7.5, and then extracted with an equal volume of chloroform containing internal standard. The content of free nicotine in e-liquid determined by GC method was 41.44 mg / g. The error between the measured value and the theoretical value is not more than 5%.

Embodiment 3

[0031] Take 1mL of e-liquid with a free nicotine concentration of 41.15mg / g and place it in a disposable e-cigarette device, and smoke on a smoking machine. The puff parameters are the international ISO deep smoking mode, and 20 puffs of e-cigarettes are collected with a Cambridge filter. Smoke aerosol. Add 5 mL of isopropanol solution containing heptadecane internal standard to the filter for collecting the aerosol, shake for 30 min, and measure the nicotine content in the aerosol by gas-phase method. The nicotine content in the aerosol is 39.44 mg / g.

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Abstract

The invention discloses a method for determining the content of free nicotine and nicotine salt in electronic cigarette liquid and smoke aerosol. The method comprises a total content determination offree nicotine and nicotine salt and a content determination of nicotine salt using gas chromatography (GC).

Description

technical field [0001] The invention belongs to the technical field of novel tobacco products, in particular to a method for determining the content of free nicotine and nicotine salt in electronic cigarette liquid and smoke aerosol. Background technique [0002] Nicotine in tobacco is essentially (over 95%) in the form of nicotine salts, typical nicotine salts in tobacco including acetate, citrate, malate and tartrate. Nicotine is an alkaloid composed of a pyridine ring and a hydrogenated pyrrole ring. It is a volatile and alkaline pyridine alkaloid, which is easy to combine with inorganic acids and various organic acids to form salts. pH is closely related. In aqueous solution there is the following equilibrium: C 10 H 14 N 2 ⇄ C 10 H 14 N 2 + ⇄ C 10 H 14 N 2 2+ ， When the pH is less than 5, it mainly exists in a double-protonated state; when the pH is between 5 and 8, it mainly exists in a single-protonated state; when the pH is greater than 10, it mainly ex...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 赵国玲龚淑果尹新强黄平邓昌健彭新辉黄建国代远刚文雅萍
Owner CHINA TOBACCO HUNAN INDAL CORP
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