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A method for the extraction and determination of tobacco-specific n-nitrosamines in mainstream cigarette smoke based on hydrophobic ion-exchange solid-phase extraction

A technology of mainstream cigarette smoke and ion exchange, applied in the field of tobacco chemical inspection, can solve the problems of swelling, affecting the enrichment and purification effect of fillers, etc. Effect

Active Publication Date: 2018-11-09
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid-phase extraction filler in this scheme is N-vinylpyrrolidone-benzenesulfonic acid copolymer, and the organic polymer filler will swell in the organic solvent, which will affect the enrichment and purification effect of the filler to a certain extent
In addition, the program did not optimize various parameters that affect the extraction effect

Method used

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  • A method for the extraction and determination of tobacco-specific n-nitrosamines in mainstream cigarette smoke based on hydrophobic ion-exchange solid-phase extraction
  • A method for the extraction and determination of tobacco-specific n-nitrosamines in mainstream cigarette smoke based on hydrophobic ion-exchange solid-phase extraction
  • A method for the extraction and determination of tobacco-specific n-nitrosamines in mainstream cigarette smoke based on hydrophobic ion-exchange solid-phase extraction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A method for extracting tobacco-specific N-nitrosamines in cigarette mainstream smoke based on hydrophobic ion-exchange solid-phase extraction of the present invention comprises the following steps:

[0062] 1) According to the regulations of GB / T 19609-2004 and ISO 4387:2000, smoke 5 cigarettes with a straight-line smoking machine, put the filter with the total particulate matter in the mainstream smoke into the container, add 15mL, 5mmol / L ammonium acetate solution, placed on an ultrasonic generator (purchased from Kunshan Ultrasound Instrument Co., Ltd., model: KQ-700DB) for ultrasonic extraction for 30min, ultrasonic power 280W, frequency 40kHz, the extract was passed through a 0.22 μm aqueous phase filter membrane, The sample crude extract is obtained, and the pH value of the sample crude extract is adjusted to 4 as the sample loading solution;

[0063] 2) Weigh 500 mg of HiCapt MCX solid-phase extraction filler into an empty solid-phase extraction column tube with...

Embodiment 2

[0086] According to the assay method described in Example 1, select other hundreds of commercially available cigarettes, and measure the content of tobacco-specific N-nitrosamines, the results are as follows: figure 2 shown.

[0087] In other embodiments of the present invention, the amount of filler in the HiCapt MCX solid-phase extraction column can also be 50 mg, 100 mg, 200 mg, 300 mg or 1000 mg, and the others are the same as in Embodiment 1. Depend on image 3 The optimization results of packing quality in HiCapt MCX solid-phase extraction column show that the quality of packing is in the range of 50-1000 mg. As the quality continues to increase, the peak area of ​​the target analyte continues to increase. When it reaches 500 mg, continue to increase the packing quality , the peak area of ​​the target analyte does not increase significantly, considering the extraction effects of all target analytes, the preferred filler mass is 500 mg.

[0088] In other embodiments of...

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Abstract

The invention relates to a method for extracting and determining specific tobacco N-nitrosamine in cigarette main-stream smoke based on hydrophobic ion exchange solid-phase extraction and belongs to the technical field of chemical tobacco examination. The method for extracting the specific tobacco N-nitrosamine in the cigarette main-stream smoke comprises the steps that a filter element capturing total particulate matter of the main-stream smoke is put in an ammonium acetate solution, filtration is performed, and a HiCapt MCX solid-phase extraction column is adopted for solid-phase extraction to obtain the specific tobacco N-nitrosamine. By adopting the method for extracting the specific tobacco N-nitrosamine in the cigarette main-stream smoke, impurities and interferents can be effectively removed, the accuracy and precision of the determining method can be improved, the relative recovery rate of the method is 92.2%-108.9%, and the intra-day precision and the inter-day precision are smaller than 4.6% and 4.2% respectively.

Description

technical field [0001] The invention relates to a method for extracting and measuring tobacco-specific N-nitrosamines in cigarette mainstream smoke based on hydrophobic ion-exchange solid-phase extraction, and belongs to the technical field of tobacco chemical testing. Background technique [0002] Tobacco-specific N-nitrosamines are produced by the reaction of amine compounds with nitrosating reagents under acidic conditions. It is also an important substance in the list of "28 harmful substances in smokeless tobacco products" of the International Agency for Research on Cancer. Therefore, accurate analysis of tobacco-specific N-nitrosamine content in mainstream cigarette smoke is of great significance for evaluating tobacco and tobacco products and ensuring the consumption safety of tobacco products. [0003] Cigarette smoke is an extremely complex mixture. More than 5,000 smoke components have been identified so far, and the content of tobacco-specific N-nitrosamines is g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/96G01N30/06G01N30/14G01N30/02G01N30/86
CPCG01N30/02G01N30/06G01N30/14G01N30/8634G01N30/96G01N2030/062G01N2030/146
Inventor 罗彦波姜兴益张洪非朱风鹏庞永强胡少东李翔宇闫瑞波陈小静
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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