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Method for determining phenolic compounds in mainstream smoke of cigarettes by supercritical fluid chromatography(SFC), gas chromatography and mass spectrum(GC-MS)

A technology of supercritical fluid and gas chromatography, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of limited peak capacity and low processing temperature, and achieve the effect of solving limited peak capacity, low processing temperature and improving analytical sensitivity

Inactive Publication Date: 2016-12-07
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a method for measuring phenolic compounds in cigarette mainstream smoke by SFC-GC-MS, the processing temperature is low, and the volatile components will not be lost during the separation process; the fractions separated by SFC are separated by GC-MS Analysis, the compounds between each section basically do not overlap, and at the same time solve the problem of limited peak capacity of GC-MS

Method used

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  • Method for determining phenolic compounds in mainstream smoke of cigarettes by supercritical fluid chromatography(SFC), gas chromatography and mass spectrum(GC-MS)
  • Method for determining phenolic compounds in mainstream smoke of cigarettes by supercritical fluid chromatography(SFC), gas chromatography and mass spectrum(GC-MS)

Examples

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Effect test

Embodiment 1

[0027] A method for SFC-GC-MS determination of phenolic compounds in cigarette mainstream smoke, comprising the following steps:

[0028] (A) Smoke collection: smoke cigarettes according to the ISO mode, use a rotary smoking machine, and use a 92mm glass fiber filter to collect the total particulate matter of 20 cigarettes;

[0029] (B) Sample extraction: add the filter piece obtained in step A into a supercritical fluid extraction column, the temperature of the extraction kettle for supercritical fluid extraction is 55°C, the extraction pressure is 300bar, static extraction is 20min, dynamic extraction is 40min, and the entrainer is Absolute ethanol, flow rate 0.01mL / min, sample obtained after supercritical fluid extraction;

[0030] (C) SFC segmentation: the extract obtained in step B enters the SFC separation system, and the supercritical fluid chromatography adopts a 10mm × 150mm, 5 μm Silica 2-EP chromatographic column, and the mobile phase is carbon dioxide / carbon dioxid...

Embodiment 2

[0035] A method for SFC-GC-MS determination of phenolic compounds in cigarette mainstream smoke, comprising the following steps:

[0036] (A) Smoke collection: smoke cigarettes according to the ISO mode, use a rotary smoking machine, and use a 92mm glass fiber filter to collect the total particulate matter of 20 cigarettes;

[0037] (B) Sample extraction: add the filter piece obtained in step A into a supercritical fluid extraction column, the temperature of the extraction kettle for supercritical fluid extraction is 55°C, the extraction pressure is 300bar, static extraction is 30min, dynamic extraction is 40min, and the entrainer is Absolute ethanol, flow rate 0.01mL / min, sample obtained after supercritical fluid extraction;

[0038] (C) SFC segmentation: the extract obtained in step B enters the SFC separation system, and the supercritical fluid chromatography adopts a 10mm × 150mm, 5 μm Silica 2-EP chromatographic column, and the mobile phase is carbon dioxide / carbon dioxid...

Embodiment 3

[0043] Same as Example 1, under the same conditions, parallel determination was performed 5 times (same batch processing), and the retention time and total peak area value were mainly investigated. The test results showed that the RSDs were all less than 4.7%. At the same time, 6 kinds of compounds were selected to carry out the standard recovery experiment. The recovery rate of the traditional method was between 86-110%, and the recovery rate of this method was between 90-105%. The recovery rate of this method was obviously high.

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Abstract

The invention discloses a method for determining phenolic compounds in mainstream smoke of cigarettes by supercritical fluid chromatography (SFC), gas chromatography and mass spectrum (GC-MS). The method comprises the following steps that: after the cigarettes are smoked, supercritical fluid is used for extracting glass-fiber filtering discs which capture total particulate matters in the mainstream smoke of the cigarettes, the supercritical fluid chromatography is used for dividing extraction liquid into multiple sections of fractions, and every section of fraction is analyzed by the gas chromatography and the mass spectrum. The method disclosed by the invention has the advantages that the problem of limited peak capacity of GC-MS is solved, the purpose that the compounds among all sections after separation are basically not overlapped can be realized. The result is satisfactory, the quantity of the separated phenolic aroma components is much more than that of direct sampling analysis, a new method is provided for determining the phenolic aroma compounds in the mainstream smoke of the cigarettes, and has significance in evaluating the hazards of smoking on health and promoting research and development of low-hazard cigarettes.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for determining phenolic compounds in cigarette mainstream smoke by supercritical fluid chromatography-gas chromatography-mass spectrometry. Background technique [0002] Phenolic substances widely exist in tobacco and smoke, and are closely related to the color, quality and physiological strength of tobacco leaves. They are an important class of compounds in the tobacco industry. Because of the high boiling point of the polyphenolic compounds in cigarettes, they will not directly enter the smoke during combustion, and most of them will decompose into simple phenolic compounds and enter the smoke. However, most of the reports about simple phenolic compounds in smoke are negative, for example: they have a strong stimulating effect on the respiratory mucosa; they cause spicy and astringent tastes, which affect the taste of cigarettes; . Therefore...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 唐石云申钦鹏刘志华刘春波杨光宇朱瑞芝王昆淼何沛张凤梅司晓喜尤俊衡王晋苏钟璧
Owner CHINA TOBACCO YUNNAN IND
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