Method for detecting urotropin in cigarette mainstream smoke through high performance liquid chromatography-tandem mass spectrum

A technology of high performance liquid chromatography and cigarette mainstream smoke, which is applied in the field of cigarette smoke to achieve good practicability, simple method and environment-friendly effect

Active Publication Date: 2015-04-15
CHINA TOBACCO JIANGSU INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As the public pays more and more attention to smoking and health problems, the harmful components in cigarette smoke are getting more and more attention. However, there are relatively few relevant reports on the detection of urotropine in smoke. In view of this, the present invention designs a A method for the detection of urotropine in mainstream cigarette smoke by high performance liquid chromatography-tandem mass spectrometry

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  • Method for detecting urotropin in cigarette mainstream smoke through high performance liquid chromatography-tandem mass spectrum

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Effect test

Embodiment 1

[0016] A method for detecting urotropine in cigarette mainstream smoke by high performance liquid chromatography-tandem mass spectrometry, specifically as follows:

[0017] According to the provisions of ISO4387:2000, capture the total particulate matter of the mainstream smoke of 20 cigarettes, put the Cambridge filter with the captured mainstream smoke total particulate matter into a 250mL bread bottle, add 40mL of acetonitrile extract to shake and extract Cambridge The filter disc was passed through a 0.45 micron filter membrane for 40 minutes, and detected by LC-MS / MS. Instrument conditions: HILIC chromatographic column, detection temperature 30°C, injection volume 2 μL, flow rate 0.25mL / min, mobile phase V (acetonitrile): V (5 mmol / L ammonium acetate solution) = 75: 25 as mobile phase for isocratic elute. The mass spectrometry conditions are: ionization mode is electrospray; scanning mode is positive ion; atomization gas 40psi; air curtain gas 10psi; auxiliary heating ga...

Embodiment 2

[0022] According to the method of embodiment 1, the minimum concentration of standard solution is continuously sampled 10 times, and its standard deviation is measured, with 3 times of standard deviation as detection limit, with 10 times of standard deviation as limit of quantification, the detection limit of urotropine It was 0.06ng / cig, and the lower limit of quantitation was 0.2ng / cig. The content of urotropine in flue-cured cigarette smoke is generally about tens of ng per stick, so this method can meet the analysis and determination of cigarette samples.

Embodiment 3

[0024] According to the method of embodiment 1, choose flue-cured tobacco type cigarette sample, measure 4 times every day simultaneously, measure 3 days altogether, calculate the intraday repeatability and daytime reproducibility of assay method, the relative standard deviation (%) in the result such as table 1 day They are 2.93, 4.26 and 4.63 respectively, and the relative standard deviation (%) between days is 3.93, so the precision of this method is better.

[0025] The precision analysis results of the method in Table 1 (unit: ng / cig)

[0026]

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Abstract

The invention claims a method for detecting urotropin in cigarette mainstream smoke through high performance liquid chromatography-tandem mass spectrum. The method comprises the steps of gathering mainstream smoke total particulate matter of 20 cigarettes according to the rule of ISO4387:2000, then putting a cambridge filter with the mainstream smoke total particulate matter into a 250mL bread bottle, adding 40 mL of ethanol extract liquor containing triethylamine to oscillate for extracting the cambridge filter for 40 minutes, then filtering through a 0.45 micron filter membrane to detect by using GC-MS / MS (Liquid Chromatography-Mass Spectrometry / Mass Spectrometry). Instrument conditions are as follows: a HILIC (Hydrophilic Interaction Chromatography) is used; the detection temperature is 30 DEG C; the sample size is 2microliter; the flow velocity is 0.25mL per minute; a ratio of a mobile phase V (acetonitrile) to V (5mmol / L ammonium acetate solution) is 75:25; the mobile phase carries out isocratic elution. Mass spectrum conditions are as follows: an ionization mode is electros spray; a scanning mode is positive ion; the atomizing gas is 40 psi; the curtain gas is 10 psi; the auxiliary trim gas is 40 psi; the collision gas is 5 psi; the ion source voltage is 4000-5000V; the ion source temperature is 250-350 DEG C. The method is simple to operate, good in separation effect, accurate to determine the nature, short in sample analysis time and high in detection sensitivity.

Description

technical field [0001] The invention belongs to the technical field of cigarette smoke, and in particular relates to a method for detecting urotropine in cigarette mainstream smoke by high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS). Background technique [0002] Urotropine is a harmful chemical component, corrosive, and can cause burns to the human body. Its melting point is 263°C. If it exceeds this melting point, it will sublimate and decompose, but it will not melt. When the temperature rises to 300°C, hydrogen cyanide is released, and when the temperature rises again, it decomposes into methane, hydrogen and nitrogen. When the human body contacts the product, it mainly causes dermatitis and eczema. Hexatropine is distributed in the mainstream and side stream smoke of cigarettes. Hexaamine in the smoke is a secondary product of the smoke, which is produced by the reaction of ammonia and formaldehyde in the smoke. The side stream smoke The cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N27/64
Inventor 沈晓晨张华庄亚东王珂清秦艳华曹毅韩开冬尤晓娟朱龙杰盛金刘琪何红梅
Owner CHINA TOBACCO JIANGSU INDAL
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