Determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke

A determination method and technology for tobacco products, applied in the field of tobacco chemical inspection, can solve the problems such as the need to improve the detection sensitivity, unfavorable simplified operation, etc., and achieve the effects of simplifying the pretreatment process, short processing time, and high detection sensitivity

Inactive Publication Date: 2017-01-11
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is only used for the determination of volatile N-nitrosamines in tobacco and smokeless tobacco products, and does not involve the determination of volatile N-nitrosamines in tobacco product emissions. and purification are completed in two steps, which is not conducive to simplifying the operation, and the detection sensitivity needs to be improved

Method used

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  • Determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke
  • Determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke
  • Determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke

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Embodiment 1

[0029] The determination method of volatile N-nitrosamines in smokeless tobacco products comprises the following steps:

[0030] 1) Pretreatment of samples

[0031] Preparation of sample extract: Weigh 1.0g of buccal (smoke-free) tobacco product (accurate to 0.1mg), put it into a 15mL centrifuge tube with stopper, and accurately add 1.0mL of sodium hydroxide solution with a concentration of 1.0mol / L , add 10mL of dichloromethane after full infiltration, put it on an ultrasonic generator (purchased from Kunshan Ultrasonic Instrument Co., Ltd., model: KQ-700DB) for ultrasonic extraction for 20min, ultrasonic power 700W, frequency 40kHz, after standing for 5min, place Centrifuge on a centrifuge for 5 minutes at a rotational speed of 10,000 rpm, remove the supernatant (ie, the organic phase) and pass it through a 0.22 μm nylon membrane to obtain the sample extract.

[0032] Dewatering and purification of the sample extract: Take 1mL of the filtrate and transfer it to a solution c...

Embodiment 2

[0047] The determination method of volatile N-nitrosamines in cigarette mainstream smoke comprises the following steps:

[0048] 1) Pretreatment of samples

[0049] Preparation of sample extract: According to the regulations of GB / T 19609-2004 and ISO 4387:2000, use a straight-line smoking machine to smoke 5 cigarettes, and place the filter disc that captures the total particle phase of mainstream smoke into the container. Add 15 mL of dichloromethane, place it on an ultrasonic generator (same as in Example 1) for ultrasonic extraction for 20 min, with ultrasonic power of 700 W, frequency of 40 kHz, and pass the extract through a 0.22 μm nylon membrane to obtain the sample extract.

[0050] Dewatering and purification of the sample extract: Take 1mL of the filtrate and transfer it to a solution containing 15mg GCB, 12.5mg PSA, 70mgMgSO 4 and 25mg NaCl in a 15mL stoppered centrifuge tube, placed on an oscillator to vibrate for 10min at a speed of 1000rpm, then placed in a cent...

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Abstract

The invention discloses a determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke and belongs to the technical field of tobacco chemical inspection. The determination method comprises the steps that graphitized carbon black, N-propyl ethylenediamine bonded silica gel, anhydrous magnesium sulfate and a sodium chloride adsorbing agent are added into a sample extracting solution, centrifugation and filtration are carried out after dispersive solid-phase extraction, and a to-be-tested solution is obtained; the to-be-tested solution is taken for gas chromatography-tandem mass spectrum analysis, the content of volatile N-nitrosamine in the to-be-tested solution is obtained with reference to a standard curve, and the content of volatile N-nitrosamine in a sample is obtained through calculation. The method is high in detection sensitivity, good in accuracy and repeatability and easy, fast and efficient to operate, the relative recovery rate is between 82.4% and 112.4%, and the intra-day precision and inter-day precision are smaller than 9.1% and 8.2% respectively.

Description

technical field [0001] The invention relates to a method for determining volatile N-nitrosamines in tobacco, tobacco products and flue gas, and belongs to the technical field of tobacco chemical inspection. Background technique [0002] N-nitrosamine is a general term for a class of compounds containing -N-NO in structure, which can be divided into volatile N-nitrosamine and non-volatile N-nitrosamine according to the difference in physical properties. Among them, volatile N-nitrosamines are a class of carcinogens that have received widespread attention. They are not only important substances in the Hoffman list and the US Food and Drug Administration's "List of Harmful and Potentially Harmful Substances in Tobacco Products and Smoke" , is also an important ingredient in the list of "28 harmful substances in smokeless tobacco products" of the International Agency for Research on Cancer. Therefore, accurate analysis of the content of volatile N-nitrosamines in the components...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/065
Inventor 罗彦波姜兴益庞永强李翔宇朱风鹏张洪非李雪刘洋
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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