Method for determining benzoapyrene in main stream smoke of cigarette by supercritical fluid chromatography-gas chromatography-mass spectrometry

A technology for mainstream cigarette smoke and supercritical fluid, applied in the field of analytical chemistry, can solve the problems of organic solvent consumption, human error, time-consuming and other problems, and achieve the effects of reducing solvent consumption, low detection limit, and improving analytical sensitivity

Active 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

It takes a lot of organic solvent and takes a long time. In addition, it is easy to cause human error due to manual operation.

Method used

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  • Method for determining benzoapyrene in main stream smoke of cigarette by supercritical fluid chromatography-gas chromatography-mass spectrometry
  • Method for determining benzoapyrene in main stream smoke of cigarette by supercritical fluid chromatography-gas chromatography-mass spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A method for measuring B[a]P in cigarette mainstream smoke by SFC-GC-MS, comprising the following steps:

[0025] (A) Smoke collection: smoke cigarettes according to the ISO mode, use a linear smoking machine, and use a 44mm glass fiber filter to collect the total particulate matter of 4 cigarettes;

[0026] (B) Sample extraction: put the filter piece obtained in step A into a 150mL conical flask with a stopper, accurately add 1mL of deuterated B[a]P solution with a pipette, accurately add 40mL of cyclohexane, and ultrasonically oscillate 30min, after filtering through a 0.4μm filter head, it is used for chromatographic analysis;

[0027] (C) SFC separation: the extract that step B obtains enters the SFC separation system, supercritical fluid chromatography adopts 10mm * 150mm, the Silica 2-EP chromatographic column of 5 μm, mobile phase carbon dioxide / methanol (90 / 10%, mass ratio ), the mobile phase flow rate is 40mL / min, the detection wavelength of the ultraviolet de...

Embodiment 2

[0031] A method for measuring B[a]P in cigarette mainstream smoke by SFC-GC-MS, comprising the following steps:

[0032] (A) Smoke collection: smoke cigarettes according to the ISO mode, use a linear smoking machine, and use a 44mm glass fiber filter to collect the total particulate matter of 2 cigarettes;

[0033] (B) Sample extraction: put the filter piece obtained in step A into a 150mL conical flask with a stopper, accurately add 1mL of deuterated B[a]P solution with a pipette, accurately add 40mL of cyclohexane, and ultrasonically oscillate 40min, after filtering through a 0.4μm filter head, it is used for chromatographic analysis;

[0034] (C) SFC separation: the extract that step B obtains enters the SFC separation system, supercritical fluid chromatography adopts 10mm * 150mm, the Silica 2-EP chromatographic column of 5 μm, mobile phase carbon dioxide / methanol (90 / 10%, mass ratio ), the mobile phase flow rate was 40mL / min, the detection wavelength of the ultraviolet d...

Embodiment 3

[0038] Same as Example 1, under the same conditions parallel determination 7 times (same batch processing), through calculating the relative standard deviation of 7 parallel determination results, the RSD that obtains B[a]P is 2.3%; The traditional GB\T21130-2007 method was used to analyze the samples, and the RSD of B[a]P was measured to be 3.6%. The results showed that the precision of the test results by the improved method was significantly higher. Such as figure 2 shown, where figure 2 a is the GC figure of the sample that the inventive method obtains, figure 2 B is the GC figure of the sample of traditional GB\T21130-2007 method, it can be seen that the method B[a]P peak of the present invention is obviously outstanding, and abundance is big, and interference peak is also obviously less and smaller, has improved analytical precision Spend. At the same time, the standard addition recovery experiment was carried out, the recovery rate of the traditional method was be...

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Abstract

The invention discloses a method for determining benzoapyrene (B[a]P) in the main stream smoke of a cigarette by supercritical fluid chromatography (SFC)-gas chromatography-mass spectrometry (GC-MS). The method comprises the following steps: adding an internal standard substance and a cyclohexane solution into a filter element for capturing total particulate matters of the main stream smoke of the cigarette after the cigarette is smoked; performing ultrasonic extraction, separating and purifying the extract with SFC; cutting fraction containing B[a]P, and analyzing with GC-MS; and fixing the quality according to the area ratio of a target peak to an isotope internal standard substance peak. According to the method, trace to-be-determined ingredient in a complex substrate can be separated from an interfering substance, interference of other substances can be eliminated, and the detection accuracy can be improved. The method has the advantages of simple pre-treatment, high separation speed, accurate quantity, low detection limit and the like.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a simple, efficient, accurate and sensitive detection method for benzo[a]pyrene in mainstream cigarette smoke. Background technique [0002] Benzo[a]pyrene (B[a]P) is a strong carcinogen in cigarette smoke and an important indicator for the safety evaluation of cigarette smoke. Content is of great significance to the monitoring of cigarette quality and safety. At present, the main methods for detecting B[a]P in mainstream cigarette smoke are GC-MS and HPLC-FLD, and the current national standard GB / T21130-2007 adopts GC / MS. The mainstream smoke components of cigarettes are very complex, the amount of B[a]P released is very small, and there are many interfering substances in cigarette smoke. Therefore, it is difficult to accurately quantitatively detect B[a]P in cigarette smoke. The samples were subjected to some pretreatment. According to the current na...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 申钦鹏唐石云刘欣刘春波杨光宇刘志华尤俊衡何沛缪明明张凤梅司晓喜王晋朱瑞芝王昆淼苏钟璧
Owner CHINA TOBACCO YUNNAN IND
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