Determination method for nicotine optical isomers in tobacco

A technology for optical isomers and determination methods, which is applied in the field of tobacco chemical analysis, can solve the problems of separation and quantitative detection of nicotine optical isomers that are not seen, and takes a long time, and achieves high sensitivity, low reagent toxicity, and repeatability. Good results

Active Publication Date: 2017-08-18
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

This method adopts multi-dimensional gas-phase gas chromatography-mass spectrometry system to realize the better separation of S-(-)-nicotine and R-(+)-nicotine, and the detection limit (LOD) of R-(+)-nicotine is 0.25%, but This method takes a long time, and it takes 56 minutes to achieve the resolution of the two chiral isomers
There are no reports on the separation and quantitative detection of nicotine optical isomers by ultra-high performance convergence chromatography tandem mass spectrometry

Method used

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  • Determination method for nicotine optical isomers in tobacco
  • Determination method for nicotine optical isomers in tobacco
  • Determination method for nicotine optical isomers in tobacco

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for determining optical isomers of nicotine in flue-cured tobacco, comprising the following steps:

[0027] (1) Sample pretreatment

[0028] According to the method of YC / T 31-1996, the moisture in the tobacco dust sample is determined;

[0029] Weigh 0.1g (accurate to 0.0001g) of smoke powder sample into a 50mL corked Erlenmeyer flask, and accurately add 10mL of 5% (v / v) HAc aqueous solution; place the Erlenmeyer flask in an ultrasonic instrument, and extract it ultrasonically for 40min with 100W power ; Filter the extract with a 0.22 μm aqueous filter membrane, take 200 μL of the filtrate and dilute it with isopropanol to a volumetric flask of 10 mL to obtain the solution to be tested;

[0030] (2) Preparation of standard working solution

[0031] The preparation of standard working solution includes the preparation of S-(-)-nicotine and R-(+)-nicotine single standard stock solution, the preparation of S-(-)-nicotine and R-(+)-nicotine mixed standard stock ...

Embodiment 2

[0051] The assay method of nicotine optical isomers in Burley tobacco comprises the following steps:

[0052] (1) Sample pretreatment

[0053] According to the method of YC / T 31-1996, the moisture in the tobacco dust sample is determined;

[0054] Weigh 0.1g (accurate to 0.0001g) of smoke powder sample into a 50mL corked Erlenmeyer flask, and accurately add 10mL of 5% (v / v) HAc aqueous solution; place the Erlenmeyer flask in an ultrasonic instrument, and extract it ultrasonically for 40min with 100W power ; Filter the extract with a 0.22 μm aqueous filter membrane, take 200 μL of the filtrate and dilute it with isopropanol to a volumetric flask of 10 mL to obtain the solution to be tested;

[0055] Other operations are the same as in Example 1, and the measurement results are shown in the following table 4, and the total ion current diagram is shown in image 3 .

Embodiment 3

[0057] A method for determining optical isomers of nicotine in oriental tobacco, comprising the following steps:

[0058] (1) Sample pretreatment

[0059] According to the method of YC / T 31-1996, the moisture in the tobacco dust sample is determined;

[0060] Weigh 0.1g (accurate to 0.0001g) of smoke powder sample into a 50mL conical flask with a stopper, and accurately add 10mL of 5% (v / v) HAc aqueous solution; place the conical flask in an ultrasonic instrument, and extract it ultrasonically for 40min at a power of 100W ; Filter the extract with a 0.22 μm aqueous filter membrane, take 500 μL of the filtrate and dilute it with isopropanol to a volumetric flask of 10 mL to obtain the solution to be tested;

[0061] Other operations are the same as in Example 1, and the measurement results are shown in the following table 4, and the total ion current diagram is shown in Figure 4 .

[0062] The assay results of 3 kinds of tobacco samples nicotine optical isomers in the embod...

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Abstract

The invention discloses a determination method for nicotine optical isomers in tobacco, and belongs to the field of tobacco chemical analysis. The determination method is characterized by extracting nicotine in a tobacco sample by adopting an acetic acid water solution, and separating and detecting two optical isomers of nicotine by using UPC<2> (Ultra Performance Convergence Chromatography)-MS (Mass Spectrometer) / MS after filtering and diluting an extracting solution. According to the determination method disclosed by the invention, low-toxicity CO2 is used as a main mobile phase, resolution and quantification of the two optical isomers can be completed within three minutes, the pretreatment operation is simple, the determination is fast, the result is accurate, the sensitivity is higher, and the determination method not only can be used for calculating the content ratio of the two optical isomers, but also is capable of realizing accurate determination of the content of the nicotine, wherein the detection limit of S-(-)-nicotine is 10.4 ng / mL, and the quantification limit is 34.6 ng / mL; the detection limit of R-(+)-nicotine is 6.6 ng / mL, and the quantification limit is 22 ng / mL; the determination method is a chromatographic determination method with highest nicotine detection efficiency at present.

Description

technical field [0001] The invention relates to a method for measuring nicotine optical isomers in tobacco, belonging to the field of chemical analysis of tobacco. Background technique [0002] Nicotine, also known as nicotine, chemically named 1-methyl-2-(3-pyridyl)pyrrolidine, is an important alkaloid present in tobacco, tobacco products and smoke, accounting for about 30% of the total alkaloids in tobacco 90%. In its molecular structure, the 2-position carbon atom on the tetrahydropyrrole ring has chirality, so nicotine has two enantiomers, namely S-(-)-nicotine and R-(+)-nicotine. The nicotine in tobacco is mainly S-(-)-nicotine, R-(+)-nicotine only accounts for about 1% of the total nicotine in tobacco raw materials, but along with the pyrolysis racemization in the combustion process, R-( +)-nicotine content can reach 2 to 3%. Many animal experiments and in vitro model experiments have shown that the metabolic processes of the two in vivo are different, and S-(-)-nic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 邓惠敏王颖杨飞唐纲岭李中皓边照阳刘珊珊范子彦
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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