Extraction and determination method of N-nitrosamine in smoke quitting product based on hydrophobic ionic exchange solid phase extraction

A technology of ion exchange and extraction method, which is applied in the direction of measuring devices, material separation, instruments, etc., which can solve the problems of inapplicable samples of smoking cessation products, affecting the enrichment and purification effect of fillers, swelling, etc., and achieves short processing time and simple operation , Improve the effect of accuracy and precision

Inactive Publication Date: 2017-06-13
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Abstract
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  • Claims
  • Application Information

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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
Moreover, traditional Chinese medicine ingredients are usually added to samples of smoking cessation products, so the sample matrix is ​​very different from that of tobacco samples, so the technical solutions in this scheme may not be applicable to samples of smoking cessation products

Method used

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  • Extraction and determination method of N-nitrosamine in smoke quitting product based on hydrophobic ionic exchange solid phase extraction
  • Extraction and determination method of N-nitrosamine in smoke quitting product based on hydrophobic ionic exchange solid phase extraction
  • Extraction and determination method of N-nitrosamine in smoke quitting product based on hydrophobic ionic exchange solid phase extraction

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Embodiment 1

[0076] The extraction method of N-nitrosamines in the smoking cessation product in this embodiment comprises the following steps:

[0077] 1) Weigh 1.0g of the filling material (accurate to 0.1mg) of ignited smoking cessation spirit, put it into a 30mL centrifuge tube with a stopper, accurately add 30mL of ammonium acetate aqueous solution with a concentration of 10mmol / L, and place it in an ultrasonic generator (purchased from Kunshan City Ultrasonic Instrument Co., Ltd., model: KQ-700DB) carries out ultrasonic treatment, ultrasonic extraction 30min, ultrasonic power 700W, frequency 40kHz, after standing for 5min, be placed on centrifuge and centrifuge 5min, centrifugal speed 10000rpm, get supernatant liquid, namely A crude extract is obtained; the pH value of the crude extract is adjusted to 4 before loading as a sample loading solution;

[0078] 2) Accurately weigh 500mg of HiCapt MCX solid-phase extraction filler into an empty solid-phase extraction column tube with a siev...

Embodiment 2

[0101] By the assay method described in embodiment 1, select several other smoking cessation products, measure the content of N-nitrosamine wherein, the result is as follows figure 2 shown (only the samples in which all 4 N-nitrosamines were detected are listed).

[0102] In other embodiments of the present invention, the pH of the crude extract can be adjusted to 3.4-11.0, further the pH of the crude extract in other embodiments of the present invention can be selected as 3.4, 6, 10.5 or 11, and the others are the same as in the implementation example 1. Since the extraction of the target analyte by the filler in the solid-phase extraction column mainly relies on hydrophobicity and cation exchange, most of the target analyte molecules exist in the protonated form when the pH is 4.0-6.0, and the cation exchange groups in the filler are in the form of negative ions. At this time, the hydrophobic interaction and cation exchange interaction between the packing material and the ...

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Abstract

The invention relates to an extraction and determination method of N-nitrosamine in a smoke quitting product based on hydrophobic ionic exchange solid phase extraction, and belongs to the technical field of tobacco chemical examination. The extraction method of N-nitrosamine in smoke quitting product based on hydrophobic ionic exchange solid phase extraction, provided by the invention, comprises the following steps of: adding the smoke quitting product into an ammonium acetate solution, the concentration of which is 5-100mmol / L, to be extracted; passing the obtained coarse extraction liquid through an activated HiCapt MCX solid extraction column; and then leaching and eluting the liquid to obtain the N-nitrosamine. The extraction method of N-nitrosamine in smoke quitting product based on hydrophobic ionic exchange solid phase extraction can effectively remove impurities and interferents, shorten the treatment time and improve the accuracy and precision of the determination method. The relative recovery rate of the method is between 92.2% and 108.9%. The within-day precision and the between-day precision are separately smaller than 4.6% and 4.2%.

Description

technical field [0001] The invention relates to an extraction and determination method of N-nitrosamines in smoking cessation products based on hydrophobic ion exchange solid-phase extraction, and belongs to the technical field of tobacco chemical inspection. 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 is of great significance to ensure the safety of product consumption. [0003] Smoking cessation products can obtain the satisfaction of ordinary cigarettes. In order to obtain this satisfaction, some samples of smoking cessation products are added with tobacco leaf components, and there will also be N-nitrosamines. However, there are no ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 罗彦波陈欢韩书磊姜兴益朱风鹏胡少东李翔宇庞永强闫瑞波陈小静付亚宁刘彤
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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