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Method for detecting cigarette mainstream flue gas benzo(a) pyrene by gel infiltration-GC/MS method

A technology of cigarette mainstream smoke and gel infiltration, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of small background, good separation effect and good effect

Active Publication Date: 2008-09-17
CHINA TOBACCO HUNAN INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to improve the separation and purification steps in the analysis process of benzo[a]pyrene in mainstream cigarette smoke, reduce sample matrix interference, and adopt a new separation and purification technology-gel permeation chromatography (GPC), through GPC The purification system effectively separates and purifies samples, thereby improving the accuracy and quantitative analysis of benzo[a]pyrene in mainstream cigarette smoke by gas chromatography-mass spectrometry, and provides an easy-to-operate, highly automated, environmentally friendly, good sample separation effect, and high sensitivity Method for the detection of benzo[a]pyrene in mainstream cigarette smoke

Method used

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  • Method for detecting cigarette mainstream flue gas benzo(a) pyrene by gel infiltration-GC/MS method
  • Method for detecting cigarette mainstream flue gas benzo(a) pyrene by gel infiltration-GC/MS method
  • Method for detecting cigarette mainstream flue gas benzo(a) pyrene by gel infiltration-GC/MS method

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Embodiment 1

[0020] The Furong brand cigarettes were smoked according to the standard conditions stipulated in YC / T29-1996. After smoking the cigarette, remove the Cambridge filter from the smoking machine, put it into a conical flask, add 40mL of cyclohexane, and perform ultrasonic extraction for 40min. Pipette 7.0 mL of the extract into a GPC sample vial and rinse with a GPC instrument. The eluent is a 1:1 mixture of cyclohexane and ethyl acetate, and the eluate is collected in a fraction bottle. Place the fraction bottle in an automatic nitrogen blower for concentration to 0.9-1.1 mL, add 10.0 μL of 9-phenylanthracene internal standard solution (concentration: 10.0 ng / μL) for GC-MS analysis. GC-MS conditions are: Agilent's DB-5MS capillary chromatographic column (30m × 0.25mm × 0.25 μ m); the injection volume is 1 μ L, split injection, split ratio 10:1 (10:1 split ratio and injection 1 μL can make the sample entering the gas chromatography and mass spectrometry less while ensuring the ...

Embodiment 2

[0022]Using cyclohexane as a solvent, configure a series of standard solutions according to the concentration range in Table 1, then carry out GC-MS analysis and detection under the above experimental conditions, and use the ratio of the peak area of ​​the component on the chromatogram to the peak area of ​​the internal standard as the response signal to establish a benzene And the standard curve of [a]pyrene, its linear relationship is shown in Table 2. The results in Table 2 show that the response signal has a significant linear correlation with the component concentration; the lowest concentration standard solution is diluted, and the detection limit is obtained according to the signal-to-noise ratio S / N=3, and the experimental results are shown in Table 2, indicating the method The detection limit is low and the method is sensitive.

[0023] Table 1 Series Standard Solution Concentration

[0024]

[0025] Table 2 Linear relationship and detection limit

[0026]

[...

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Abstract

The invention provides a method for detecting the benzo[a]pyrene in the main stream smoke of cigarette using gel permeation-GC-MS. The cambridge filter disc is dismounted from the smoking machine and mounted into a cone flask with plug and then is subjected to ultrasonic extraction in ultrasonic after adding cyclohexane. The extract liquid is moved into a GPC sample bottle and is leached using the cyclohexane-ethyl acetate mixed liquor and the leaching liquid is collected and concentrated in an automatic concentrating device. The internal standard solution is added into the concentrated liquid and analyzed by GC -MS apparatus to quantitate based on component peak area and internal standard peak area. The condition of the GC-MS is that: DB-5MS capillary chromatographic column; split stream or not split stream sampling; N2 as carrier gas; temperature of the injection port:230-260 degree; temperature programming. The invention has high automaticity, friend environment, easy operation, less interference, high sensitivity and good accuracy.

Description

technical field [0001] The invention relates to a method for detecting benzo[a]pyrene, in particular to a method for detecting benzo[a]pyrene in mainstream smoke of cigarettes. Background technique [0002] Polycyclic aromatic hydrocarbons (PAHs) are the earliest discovered carcinogens with a large number and wide distribution, among which benzo[a]pyrene (B[a]P) is one of more than 200 carcinogens discovered Representative compounds with strong carcinogenicity among fused aromatic hydrocarbons. Cigarettes can produce a small amount of benzo[a]pyrene during the combustion process. Therefore, the determination of benzo[a]pyrene content in mainstream cigarette smoke is of great significance to the research on smoking and health. [0003] Since the 1960s, a large number of studies have been carried out at home and abroad on the extraction, purification, separation and detection of benzo[a]pyrene in mainstream cigarette smoke. The content of benzo[a]pyrene in cigarette smoke is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/88
Inventor 吴名剑练文柳蒋腊梅吴银菊庹苏行胡念念
Owner CHINA TOBACCO HUNAN INDAL CORP
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