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Method for measuring trace alkaloids and nitrosamines in oral tobacco products

A determination method and alkaloid technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex matrix and difficult extraction, and achieve the effects of strong selectivity, reduced impurity interference, and high accuracy

Pending Publication Date: 2019-07-05
CHINA TOBACCO GUIZHOU IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] So far, there are few reports on the content detection of trace alkaloids in snus, and the determination method of tobacco-specific nitrosamines in snus mainly refers to the method of traditional cigarettes, using HAC solvent extraction and liquid chromatography-tandem Mass spectrometry, but there are obvious differences between snus and traditional cigarettes. For example, gum-based snus contains gum base, which brings certain difficulties to the extraction, and the matrix is ​​more complex, so traditional liquid chromatography-tandem mass spectrometry is not necessarily Very suitable; In addition, the method for simultaneous determination of trace alkaloids and tobacco-specific nitrosamines in snus has not been reported

Method used

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  • Method for measuring trace alkaloids and nitrosamines in oral tobacco products
  • Method for measuring trace alkaloids and nitrosamines in oral tobacco products
  • Method for measuring trace alkaloids and nitrosamines in oral tobacco products

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Experimental program
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Effect test

Embodiment 1

[0037] Such as Figure 11 As shown, the assay steps of trace alkaloids and nitrosamines in the snus of the present embodiment include:

[0038] 1) Cut the gum-based snus into sheet-like objects with a thickness of 0.5-1.0 mm, weigh the analysis samples with an analytical balance, mark them as sample 1 and sample 2, and each sample is about 1.0 g.

[0039] Put sample 1 and sample 2 into 10mL extraction kettles respectively, add 200μL of internal standard and 20mL of methanol as the extraction solvent in sequence, and then use the accelerated solvent extraction method to repeat the extraction twice, each time for 5min, the extraction temperature is 50 °C; then, rinse with 5 mL of methanol, and collect the extract. Among them, the internal standards are Mesmin-D4, Cotinine-D3, Nicotriptyline-D9, NNK-D4, NNN-D4, NAB-D4 and NAT-D4, and the internal standard concentration is 10ug / mL.

[0040] After standing for a period of time, take about 1.5mL supernatant and add it to a 2mL cen...

Embodiment 2

[0050] Embodiment 2 methodological investigation

[0051] 1) Standard curve

[0052] Using acetonitrile as solvent, a series of standard solutions of different concentrations of trace alkaloids and tobacco-specific nitrosamines were prepared, and the above instrument conditions were used for UPLC-HR-MS analysis. Then adopt the internal standard method to quantify (internal standard is: mesmin-D4, cotinine-D3, nicotriptyline-D9, NNK-D4, NNN-D4, NAB-D4 and NAT-D4), with each target The peak area ratio of the target substance and its internal standard is the ordinate (Y), and the concentration of each target substance is the abscissa (X, ng / mL) for regression analysis to obtain 6 trace alkaloids (pseudobasine, nornicotine, massine, etc. Table 2 shows the regression equations and correlation coefficients of 4 kinds of tobacco-specific nitrosamines (NNK, NNN, NAB and NAT) and N-formyl nornicotine, cotinine, nicotriptyline and N-formyl nornicotine.

[0053] It can be seen from Tab...

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Abstract

The invention provides a method for measuring trace alkaloids and nitrosamines in oral tobacco products. The method includes the following steps that: a) oral tobacco products are sliced, and are added into to an extraction solvent and a deuterated isotope internal standard, extraction is performed with an accelerated solvent extraction method, an extract liquid is collected; b) the extract liquidand a QuECHERS reagent are subjected to vortex mixing for 1-3min, centrifuging is performed at a speed of 9000-11000 rpm for 3-7min, so that a supernate can be obtained; and c) a UPLC-HR-MS method isadopted to perform quantitative analysis on trace alkaloids and specific nitrosamines for the cigarettes in the supernate. With the method disclosed by the invention adopted, 6 trace alkaloids, namely, neonicotine, nornicotine, myosmine, cotinine, nicotelline and N-formyl nornicotine and four specific nitrosamines, namely NNN, NNK, NAT and NAB in the main stream smoke of cigarettes can be measured simultaneously. The method has the advantages of high sensitivity, high accuracy and high selectivity, and is suitable for the rapid determination of trace alkaloids and nitrosamines in batched gum-base oral tobacco products.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical testing of chemical components of tobacco products, and in particular relates to a method for measuring trace alkaloids and nitrosamines in snus. Background technique [0002] Snus is a type of smokeless tobacco product used through the mouth. From the perspective of ingredients, snus is composed of tobacco powder / tobacco extract and added inorganic salts, spices, water, humectants and other ingredients. Snus is a moist or semi-moist powdered tobacco product. Snus does not go through the combustion process, it is directly consumed by the mouth, does not produce smoke, and has almost no impact on the public and the environment. However, the tobacco powder / cut tobacco / tobacco extract added to snus often contain a small amount of trace alkaloids (such as pseudobasine, nornicotine, mesmin, cotinine, nicotriptyline, and N-formazine) acyl nornicotine) and tobacco-specific nitrosamines. ...

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 张小涛刘剑张丽阮艺斌王维维姬厚伟万强
Owner CHINA TOBACCO GUIZHOU IND
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