Method for determining total nicotine in nicotine salt-containing electronic cigarette liquid and aerosol

A technology of electronic cigarette liquid and aerosol, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of incomplete detection, misleading consumers, and inability to measure the content of nicotine salts.

Pending Publication Date: 2022-03-29
CHINA TOBACCO HUNAN INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cai Junlan et al. used gas chromatography to establish a method for the determination of nicotine, 1,2-propanediol and glycerol in electronic cigarette liquid. This method is easy to operate and suitable for the determination of large quantities of samples, but it cannot determine the content of nicotine salts.
The prior art CN104062385A adopts the method of GC-FID to measure the nicotine content in the electronic cigarette, but under this operating condition, it is also impossible to measure the total nicotine content in the smoke containing nicotine salt, only free nicotine can be measured Alkali content
Similarly, the inventors of the present application found in the previous research (CN11323490A) in the process of measuring the content of free nicotine and nicotine salt in e-cigarette liquid and smoke aerosol by gas phase method that the temperature of the sample injection place is between 100-220°C Can not effectively measure the content of nicotine in nicotine salt
The main reason is that part of the nicotine salt is not completely cracked under the measurement conditions described, so it cannot be completely detected
[0004] However, most of the nicotine in the current nicotine-containing electronic cigarette liquid exists in the form of nicotine salt. If the nicotine content is still determined by the existing method, it is impossible to give an accurate nicotine content. It will be misleading to consumers, so there is a need for an accurate method for determining the nicotine content in e-liquids containing nicotine salts

Method used

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  • Method for determining total nicotine in nicotine salt-containing electronic cigarette liquid and aerosol
  • Method for determining total nicotine in nicotine salt-containing electronic cigarette liquid and aerosol
  • Method for determining total nicotine in nicotine salt-containing electronic cigarette liquid and aerosol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Instruments and instrument working conditions:

[0037] The chromatographic column is DB-ALC1 (30m×0.32mm×0.118μm) capillary gas chromatography column.

[0038] Preferably, the instrument conditions in the GC-FID method described in step S3: column oven temperature: 170°C; detector temperature: 275°C; carrier gas: helium (≥99.999%), constant flow mode flow rate: 1.0mL / min; compressed air flow rate: 400.0mL / min; hydrogen flow rate: 40.0mL / min; makeup gas helium flow rate: 25.0mL / min; injection volume: 1μL, split injection; heating program: 90°C (1min) , 15°C / min; 120°C (0min), 40°C / min; 240°C (4min).

[0039] Described detection comprises the following steps:

[0040] S1. Configuration of extractant: Pipette a certain amount of n-heptadecane and dilute it in isopropanol solution and shake it up as the extractant. The concentration range of n-heptadecane diluted in isopropanol solution is 0.01mg / mL ~0.1mg / mL;

[0041] S2. Prepare standard series solutions of nicotine...

Embodiment 2

[0046] Apply the method of the present invention to measure the total nicotine content in the electronic cigarette liquid containing nicotine salt, wherein the nicotine salt in the electronic cigarette liquid is: nicotine tartrate (the molar ratio of nicotine to acid is 1:1) , nicotine phosphate (the molar ratio of nicotine to acid is 1:1), nicotine oxalate (the molar ratio of nicotine to acid is 1:1), nicotine oxalate (the molar ratio of nicotine to acid is 1:1), nicotine oxalate (the molar ratio of nicotine to acid is 1:1), 2:1), nicotine malate (the molar ratio of nicotine to acid is 1:1), nicotine malate (the molar ratio of nicotine to acid is 2:1). Among them, isopropanol was selected as the extractant, n-heptadecane was used as the internal standard, the temperature of the injection port was 300°C, the split ratio was 5:1, 15:1, and 25:1, and the concentration of nicotine at the injection port was 0.001mg / mL. Such as figure 2 As shown, most of the e-cigarette liquids...

Embodiment 3

[0048] Apply the method of the present invention to measure the total nicotine content in the electronic cigarette liquid containing nicotine salt, wherein the nicotine salt in the electronic cigarette liquid is: nicotine tartrate (the molar ratio of nicotine to acid is 1:1) , nicotine phosphate (the molar ratio of nicotine and acid is 1:1), nicotine benzoate (the molar ratio of nicotine and acid is 1:1), nicotine oxalate (the molar ratio of nicotine and acid is 1:1), The molar ratio is 1:1), nicotine oxalate (the molar ratio of nicotine and acid is 2:1), nicotine malate (the molar ratio of nicotine and acid is 1:1), nicotine malic acid Salt (2:1 molar ratio of nicotine to acid). Among them, isopropanol was selected as the extractant, n-heptadecane was used as the internal standard, the temperature of the injection port was 300°C, the split ratio was 25:1, and the concentration of nicotine at the injection port was 0.0005mg / mL, 0.001mg / mL, 0.002 mg / mL, 0.008mg / mL. Such as ...

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Abstract

The invention discloses a method for accurately determining total nicotine in electronic cigarette liquid and aerosol containing nicotine salt. According to the method, the content of the total nicotine in the electronic cigarette liquid containing the nicotine salt is measured through a gas phase method (GC-FID), the influence of the temperature of a sample inlet, the split ratio and the nicotine concentration of the sample inlet on the content of the total nicotine is studied in detail, the temperature of the gas phase sample inlet is 250-300 DEG C, the split ratio is 5-50: 1, and the content of the nicotine in the electronic cigarette liquid containing the nicotine salt is measured. When the nicotine concentration of a sample inlet is smaller than or equal to 0.001 mg/mL, the total nicotine content in the electronic cigarette containing the nicotine salt can be accurately measured.

Description

technical field [0001] The invention belongs to the field of nicotine detection and relates to a method for measuring total nicotine in electronic cigarette liquid and aerosol containing nicotine salt. Background technique [0002] E-cigarettes are devices that atomize smoke liquid by means of electric heating to generate aerosols for consumers to smoke. Due to the low atomization temperature and the release of harmful components is much lower than that of traditional cigarettes, it has been favored by consumers in recent years. In order to satisfy consumers, a certain proportion of nicotine is usually added to e-cigarette liquids, but there are two problems. ① Nicotine mainly adheres to the mouth and upper respiratory tract, resulting in a strong sense of irritation and choking sensation when smoking ; ② Long-term storage of nicotine is easy to be oxidized, resulting in a reduced sense of satisfaction when smoking. For this reason, in 2015, Pax Labs used benzoic acid as a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 赵国玲张博龚淑果尹新强邓昌健黄平彭新辉
Owner CHINA TOBACCO HUNAN INDAL CORP
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