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Method for detecting urotropin in cigarette mainstream smoke through gas chromatography-tandem mass spectrum

A technology of cigarette mainstream smoke and tandem mass spectrometry, which is applied in the field of cigarette smoke, and achieves the effects of simple method, wide application and accurate measurement

Active Publication Date: 2014-05-21
CHINA TOBACCO JIANGSU INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 GC-MS / MS

Method used

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  • Method for detecting urotropin in cigarette mainstream smoke through gas chromatography-tandem mass spectrum
  • Method for detecting urotropin in cigarette mainstream smoke through gas chromatography-tandem mass spectrum
  • Method for detecting urotropin in cigarette mainstream smoke through gas chromatography-tandem mass spectrum

Examples

Experimental program
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Effect test

Embodiment 1

[0020] A method for detecting urotropine in cigarette mainstream smoke by gas chromatography-tandem mass spectrometry, specifically as follows:

[0021] According to the provisions of ISO4387:2000, capture the total particulate matter of the mainstream smoke of 20 cigarettes, put the Cambridge filter disc that has captured the total particulate matter of the mainstream smoke into a 250mL bread bottle, add 40mL of ethanol containing triethylamine Shake the extract to extract the Cambridge filter for 40 minutes, accurately pipette 20mL of the extract through the activated silica gel column, first rinse the column with 30mL of dichloromethane, discard the eluent, then rinse the column with 40mL of methanol, After collecting the eluent and concentrating it to 1 mL, add 50 μL of 10 mg / L internal standard solution accurately, and use GC-MS / MS for detection.

[0022] Instrument conditions: chromatographic column: HP-5 MS (30m×0.25 mm×0.25μrn); inlet temperature: 220°C; temperature pr...

Embodiment 2

[0031] According to the method of Example 1, the lowest concentration of the standard solution was continuously injected 10 times, and the standard deviation was measured, with 3 times the standard deviation as the detection limit and 10 times the standard deviation as the limit of quantification. The results are shown in Table 1. The detection limit of the product was 0.46 ng / cig, and the lower limit of quantification was 1.54 ng / cig. The content of urotropine in flue-cured cigarette smoke is generally around 30 ng / cig, so this method can meet the analysis and determination of cigarette samples.

[0032] Table 1 Analysis of the results of 10 injections of the lowest standard sample

[0033]

Embodiment 3

[0035] According to the method of Example 1, select the flue-cured tobacco type cigarette samples, and measure 4 times a day at the same time, measure 3 days in total, calculate the intra-day repeatability and day-to-day reproducibility of the determination method, the results are shown in Table 2. The relative standard deviation (%) within the day They are 4.33, 3.72 and 3.98 respectively, and the relative standard deviation (%) between days is 4.35, so the precision of this method is good.

[0036] Table 2 Precision analysis results of the method (unit: ng / cig)

[0037]

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Abstract

The invention discloses a method for detecting urotropin in cigarette mainstream smoke through gas 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, accurately taking out 20mL of the extract liquor to pass through an activated silica gel columella, washing the columella by using 30ml of dichloromethane firstly, dropping leacheate, then washing the columella by using 40mL of methyl alcohol, collecting the leacheate to concentrate to 1mL, accurately adding 50 microliters of 10mg / L internal standard solution to detect by using GC-MS / MS (Gas Chromatography-Mass Spectrometry / Mass Spectrometry). According to the method, the GC-MS / MS is used for detecting the urotropin in the cigarette side stream smoke; a multi-reaction monitoring mode is adopted for determining the nature; the method is capable of effectively improving the qualitative accuracy and sensitivity of the method, suitable for the detection of urotropin in various types of cigarette side stream smoke, wide in application and capable of accurately detecting; meanwhile, the method is simple, environment-friendly, and good in practicability.

Description

technical field [0001] The invention belongs to the technical field of cigarette smoke, and in particular relates to a gas chromatography-tandem mass spectrometry (GC-MS / MS) method for detecting urotropine in cigarette mainstream smoke. 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 content in it is higher tha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 沈晓晨张华庄亚东秦艳华朱怀远王晨辉李朝建张媛刘献军廖惠云王珂清刘琪
Owner CHINA TOBACCO JIANGSU INDAL
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