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Extraction and determination method of special N-nitrosamine of tobacco in tobacco or tobacco product based on hydrophobic ionic exchange solid phase extraction

A technology of tobacco products and ion exchange, applied in the field of tobacco chemical inspection, can solve problems such as affecting the enrichment and purification effect of fillers, swelling and other problems, achieve good purification effect, improve accuracy and precision, and remove impurities and interfering substances. Effect

Inactive Publication Date: 2017-06-13
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • 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

Method used

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  • Extraction and determination method of special N-nitrosamine of tobacco in tobacco or tobacco product based on hydrophobic ionic exchange solid phase extraction
  • Extraction and determination method of special N-nitrosamine of tobacco in tobacco or tobacco product based on hydrophobic ionic exchange solid phase extraction
  • Extraction and determination method of special N-nitrosamine of tobacco in tobacco or tobacco product based on hydrophobic ionic exchange solid phase extraction

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Effect test

Embodiment 1

[0074] In this embodiment, the method for extracting tobacco-specific N-nitrosamines based on hydrophobic ion exchange solid-phase extraction in tobacco or tobacco products comprises the following steps:

[0075] 1) Weigh 1.0 g of tobacco (accurate to 0.1 mg), put it into a 30 mL centrifuge tube with a stopper, accurately add 30 mL of ammonium acetate aqueous solution with a concentration of 10 mmol / L, and place it in an ultrasonic generator (purchased from Kunshan Ultrasound Instrument Co., Ltd., Model: KQ-700DB) for ultrasonic treatment, ultrasonic extraction for 30min, ultrasonic power 700W, frequency 40kHz, after standing for 5min, placed on a centrifuge for 5min, centrifugal speed 10000rpm, take the supernatant to obtain the crude extract; The pH value of the extract was adjusted to 4 before loading as the loading solution;

[0076] 2) Accurately weigh 500mg of HiCapt MCX solid-phase extraction filler into an empty solid-phase extraction column tube with a sieve plate, be...

Embodiment 2

[0100] According to the assay method described in Example 1, select other hundreds of tobacco or tobacco products, and measure the content of tobacco-specific N-nitrosamines, the results are as follows: figure 2 shown.

[0101] 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 filler in the HiCaptMCX solid-phase extraction column extracts the target analyte mainly by hydrophobic 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 group in the filler In the form of negative ions, the hydrophobic interaction and cation exchange force between the filler and the target analyte are strong at this time, so it has the best extraction effect. Such as ima...

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Abstract

The invention relates to an extraction and determination method of special N-nitrosamine of tobacco in tobacco or a tobacco product based on hydrophobic ionic exchange solid phase extraction and belongs to the technical field of tobacco chemical examination. The extraction method, provided by the invention comprises the following steps of: adding the tobacco or the tobacco 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 special N-nitrosamine of tobacco in tobacco or the tobacco product based on hydrophobic ionic exchange solid phase extraction provided by the invention 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 a method for extracting and measuring tobacco-specific N-nitrosamines in tobacco or tobacco 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 in tobacco and tobacco products is of great significance for evaluating tobacco and tobacco products and ensuring the consumption safety of tobacco products. [0003] There are two earliest established detection methods for tobacco-specific N-nitrosamines in tobacco or tobacco products: the first method is that the sample is ...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88G01N30/86
Inventor 罗彦波姜兴益庞永强朱风鹏张洪非胡少东李翔宇陈小静闫瑞波
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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