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Method for measuring trace alkaloids and nitrosamines in cigarette filters

A determination method and cigarette filter technology, which are applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of complicated and time-consuming pretreatment, and achieve the effect of simplifying the sample pretreatment procedure, strong selectivity, and reducing the interference of impurities

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

AI Technical Summary

Problems solved by technology

The separation effect and chromatographic reproducibility of gas chromatography-mass spectrometry are good, but the pretreatment of GC / MS method is more complicated and time-consuming; liquid chromatography-tandem mass spectrometry is more suitable for complex systems due to its high sensitivity and strong selectivity Separation and Analysis of Medium and Trace Compounds (TSNAs)
However, there is no report on the simultaneous determination of trace alkaloids and tobacco-specific nitrosamines in cigarette filters by liquid chromatography-tandem mass spectrometry or liquid chromatography-high resolution mass spectrometry

Method used

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  • Method for measuring trace alkaloids and nitrosamines in cigarette filters
  • Method for measuring trace alkaloids and nitrosamines in cigarette filters
  • Method for measuring trace alkaloids and nitrosamines in cigarette filters

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Experimental program
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Effect test

Embodiment 1

[0038] Such as Figure 12 As shown, the assay steps of trace alkaloids and nitrosamines in the cigarette filter of the present embodiment are:

[0039] 1) Collect test samples: take 2 smoked cigarette filters as test samples, and mark them as filter 1 and filter 2.

[0040] 2) Sample pretreatment

[0041] Remove the unburned cut tobacco, cut it into four parts longitudinally, put it into a 10mL extraction kettle, add 200μL of internal standard and 20mL of 40% methanol solution as the extraction solvent in sequence, and then use the accelerated solvent extraction method to repeat the extraction twice , extracting for 5 minutes each time, and the extraction temperature was 50° C.; then, rinse with 5 mL of methanol, and collect the extract. Among them, the internal standards are diene nicotine-D3, pseudobasine-D4, cotinine-D3 and nicotriptyline-D9, and the concentration of the internal standard is 10ug / mL.

[0042] After standing for a period of time, take about 1.5mL supernat...

Embodiment 2

[0052] Embodiment 2 methodological investigation

[0053] 1) Standard curve

[0054] 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: diene nicotine-D3, mesmin-D4, cotinine-D3 and nicotriptyline-D9), take the peak area ratio of each target substance and its internal standard as vertical Coordinate (Y), the concentration of each target is the abscissa (X, ng / mL) for regression analysis, and 7 kinds of trace alkaloids (diene nicotine, pseudobasine, nornicotine, mesmin, alternative Ning, Nicotriptyline and N-formyl nornicotine), four tobacco-specific nitrosamines (NNK, NNN, NAB and NAT) regression equations and their correlation coefficients are shown in Table 2.

[0055] It can be seen from Table 2 that the linear relationship...

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Abstract

The invention provides a method for measuring trace alkaloids and nitrosamines in cigarette filters. The method includes the following steps that: a) smoked cigarette filters are acquired, and are longitudinally cut, the cut cigarette filters are added to an extraction solvent and a deuterated isotope internal standard, extraction is performed with an accelerated solvent extraction method, and anextract liquid is collected; b) the extract liquid is added into a QuECHERS kit and is subjected to vortex mixing for 1-3 minutes, and centrifuging is performed at the speed of 9000-11000 rpm for 3-7minutes, and a supernate can be obtained; and c) a UPLC-HR-MS method is adopted to perform quantitative analysis on trace alkaloids and specific nitrosamines for cigarettes in the supernate. With themethod disclosed by the invention adopted, 7 trace alkaloids, namely, nicotyrine, 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 the cigarettes can be measured simultaneously. The method has the advantages of high sensitivity, a high accuracy and high selectivity, and is suitable for the rapid determination of trace alkaloids and nitrosamines in batch cigarette filters.

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 cigarette filters. Background technique [0002] Tobacco trace alkaloids are one of the most important chemical components in tobacco and cigarette smoke. The content of trace alkaloids can affect the aroma, concentration and irritation of cigarettes. At the same time, tobacco trace alkaloids are also the source of tobacco-specific nitrosamines (TSNAs). precursor substances. The U.S. FDA has listed such as N-nitroso nornicotine (NNN), 4-(methylnitrosamine)-1-(3-pyridyl)-1-butanone (NNK), N-nitroso Four TSNAs including neonicotinoid (NAT) and N-nitrosobasine (NAB) were included in the list of harmful ingredients. During the smoking process of cigarettes, cigarette filters will retain some tobacco trace alkaloids and TSNAs. Accurate determination...

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 张小涛刘剑张丽姬厚伟阮艺斌王维维万强
Owner CHINA TOBACCO GUIZHOU IND
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