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GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes

A technology for cigarette mainstream smoke and benzo, applied in the field of determination of three polycyclic aromatic hydrocarbons

Active Publication Date: 2013-08-21
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0006] GC / MS method to measure polycyclic aromatic hydrocarbons in cigarette mainstream smoke generally uses organic solvents such as n-hexane or cyclohexane containing internal standard to extract the total particle phase of smoke The extract was purified with a silica gel solid-phase extraction column. After the eluate was concentrated, it was analyzed by GC / MS and quantified by the selected ion monitoring (SIM) mode, which has high recovery rate, high sensitivity, good repeatability, and accurate quantification, etc. characteristics, but the cumbersome solid-phase extraction purification process and concentration process are required in the sample pretreatment process, which is time-consuming and laborious, and it was found in the GC / MS detection process of polycyclic aromatic hydrocarbons in the mainstream smoke of cigarettes with tar content less than 1 mg / cig, The content of benzo[a]pyrene is mostly lower than 1 ng / cig, and the GC / MS chromatographic peak of benzo[a]pyrene is low at this time, which brings certain difficulties to the quantification

Method used

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  • GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes
  • GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes
  • GC-MS/MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0039] 1. Instruments and reagents:

[0040] Targets: benzo[a]anthracene, quinone and benzo[a]pyrene, internal standard: d 12 -BaP, all standard products; acetone, ethyl acetate, chromatographic pure reagents.

[0041] American Thermo Fisher TSQ Quantum GC gas chromatography-triple quadrupole tandem mass spectrometer; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g); American Labnet VtexMixer VX200 oscillator; German Sigma high-speed refrigerated centrifuge.

[0042] 2. Sample processing:

[0043] After collecting the particulate matter of 5 cigarettes according to ISO 3308:2000 method, remove the Cambridge filter;

[0044] Accurately add 10 mL of ethyl acetate solvent and 100 μL of internal standard solution, and shake and extract on a shaker at 200 rpm for 30 min;

[0045] Take 5 mL of the extract and add it to a matrix-dispersed solid-phase extraction centrifuge tube (containing 900 mg MgSO 4 , 250 mg PSA), vortexed at 2000 rpm for 2 min on a vortex mixer,...

example 2

[0055] As described in Example 1, another brand of cigarette sample B was selected, and the contents of benzo[a]anthracene, quinone and benzo[a]pyrene were measured in Table 4.

[0056] Table 4 Detection results of benzo[a]anthracene, quinone and benzo[a]pyrene in cigarette B

[0057] serial number name Content of target substance (ng / cig) 1 Benzo[a]anthracene 2.80 2 bend 2.62 3 Benzo[a]pyrene 1.25

example 3

[0059] As described in Example 1, another brand of cigarette sample C was selected, and the measured contents of benzo[a]anthracene, quinone and benzo[a]pyrene in the sample are shown in Table 5.

[0060] table 5 Determination results of benzo[a]anthracene, quinone and benzo[a]pyrene in cigarette C

[0061] serial number name Content of target substance (ng / cig) 1 Benzo[a]anthracene 14.46 2 bend 15.65 3 Benzo[a]pyrene 8.57

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Abstract

The invention discloses a GC-MS / MS (Gas chromatography-tandem mass spectrometry) method for simultaneously analyzing benzo [a] BaA, chrysene and benzo [a] BaP in main stream smoke of cigarettes. The method is characterized by comprising the following steps of: taking out a Cambridge filter disc catching granule phase objects of main stream smoke of cigarettes, adding ethyl acetate and an internal standard, carrying out vibrating extraction, carrying out dispersive solid-phase extraction (d-SPE) on extracting liquid, then, carrying out nitrogen-blowing concentration on supernatant, and measuring by using GC-MS / MS. The method provided by the invention overcomes the deficiency that the existing pretreatment is tedious. A sample pretreatment method and an instrument detection condition are optimized, aiming at the granule phase objects of main stream smoke of cigarettes; the matrix disperse solid phase extraction (d-SPE) is selected to be used as a purification measure in purifying treatment; compared with a national standard method solid phase extract phase, the operation is simple, and the price is low; and the method provided by the invention has the advantages of accurate operation, high sensitivity and good repeatability.

Description

[0001] technical field [0002] The invention belongs to the technical field of detection of harmful substances in cigarette smoke, and mainly relates to three polycyclic compounds such as benzo[a]anthracene (BaA), chrysene and benzo[a]pyrene (BaP) in cigarette mainstream smoke. Determination techniques of aromatic hydrocarbons. [0003] Background technique [0004] Benzo[a]pyrene and other polycyclic aromatic hydrocarbons are one of the main harmful substances in mainstream cigarette smoke, and have strong carcinogenic effects. The weight analysis of previous animal or human toxicology studies shows that the most carcinogenic substances in tobacco are TSNAs and PAHs have always been the hotspots of people's research. [0005] The current standard method for the determination of benzo[a]pyrene in mainstream cigarette smoke is "GB / T 21130-2007 Determination of benzo[a]pyrene in total particulate matter in cigarette smoke". The main method for analyzing BaP is GC / MS, and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 唐纲岭陈晓水边照阳陈再根杨飞刘珊珊刘洋张洪非李中皓胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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