GC-MS (Gas Chromatography-Mass Spectrometer)/MS (Mass Spectrometer) method for simultaneously analyzing four tobacco-specific nitrosamines (TSNAs) in main stream smoke of cigarette
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A technology for cigarette mainstream smoke and nitrosamines, which is applied to the analysis of materials, material separation, measuring devices, etc.
Active Publication Date: 2013-09-11
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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[0004] For the determination of tobacco-specific N-nitrosamines in the total particulate matter of mainstream smoke by GC-TEA method, since the thermal energy analyzer only detects nitrosamines and nitrites The response is a specific detector, so it has quite high selectivity and sensitivity, but the disadvantage of this method is that there are many purification steps, long analysis time, and for flue-cured tobacco with extremely low N-nitrosamine content in tobacco , the sensitivity of GC-TEA is slightly insufficient
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example 1
[0036] 1. Instruments and reagents:
[0037] Targets: NNN, NAT, NAB, NNK, internal standard: d 4 -NNN,d 4 -NAT,d 4 -NAB,d 4 -NNK, both are standard products; acetone, ethyl acetate, are chromatographic pure reagents.
[0038] 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.
[0039] 2. Sample handling:
[0040] After collecting the particulate matter of 5 cigarettes according to the ISO 3308:2000 method, remove the Cambridge filter;
[0041] Accurately add 10 mL of ethyl acetate and 100 μL of internal standard solution, shake and extract on the shaker at 200 rpm for 30 min;
[0042] 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), shaken at 2000 rpm for 2 min on a vortex mixer,...
example 2
[0052] As described in Example 1, another brand of cigarette sample B was selected, and the contents of benzopyrene and NNK in the sample were measured in Table 4.
[0053] Table 4 Detection results of benzopyrene and NNK in cigarette B
[0054] serial number name Content of target substance (ng / cig) 1 NNN 4.10 2 NAB 11.16 3 NAT 1.28 4 NNK 5.78
example 3
[0056] As described in Example 1, another brand of cigarette sample C was selected, and the contents of benzopyrene and NNK in the sample were measured in Table 5.
[0057] table 5 Detection results of benzopyrene and NNK in cigarette C
[0058] serial number name Content of target substance (ng / cig) 1 NNN 41.39 2 NAB 32.26 3 NAT 5.73 4 NNK 22.43
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Abstract
The invention discloses a GC-MS / MS (Gas Chromatography-Mass Spectrometer) / MS (Mass Spectrometer) method for simultaneously analyzing four tobacco-specific nitrosamines (TSNAs) in main stream smoke of a cigarette. The method is characterized by comprising the steps of: adding ethyl acetate and an internal standard substance after taking out a Cambridge filter on which main stream smoke particulate phase substances are captured; getting an extract liquor after vibrating extraction and carrying out dispersive solid-phase extraction (d-SPE) on the extract liquor; then getting the supernatant liquor and carrying out nitrogen flushing concentration on the supernatant liquor; and measuring by a GC-MS / MS method. According to method disclosed by the invention, the shortcoming of complex treatment an existing method is overcome, and the pretreatment method of a sample and the instrument detection conditions are optimized aiming at the main stream smoke particulate phase substances in the cigarette. Compared with the prior art, the method disclosed by the invention has the following good effects that four TSNAs are simultaneously extracted by using ethyl acetate in pretreatment of the sample, so the good extraction efficiency is realized. Compared with the national standard method, the method disclosed by the invention has the effect that the use amount of organic solvent can be reduced by tens of times (260ml of dichloromethane is needed for measuring the TSNAs according to the national standard), and has the advantages of accuracy in operation, high sensitivity and good repeatability.
Description
technical field [0001] The invention belongs to the technical field of detecting harmful substances in cigarette smoke, and mainly relates to a technique for measuring four kinds of tobacco-specific nitrosamines, such as NNN, NAT, NAB and NNK, in mainstream smoke of cigarettes. Background technique [0002] Tobacco-specific N-nitrosamines (TSNAs) are a class of tobacco-specific harmful substances in mainstream cigarette smoke. They have strong carcinogenic effects. NNN and NNK are defined as Group 1-confirmed human carcinogens by the International Organization for Research on Cancer. The weight analysis of previous animal or human toxicology studies shows that the strongest carcinogenic effects in tobacco are TSNAs and PAHs, which have always been the hotspots of people's research. [0003] The current national standard method for tobacco-specific N-nitrosamines is "GB / T 23228-2008 Determination of tobacco-specific N-nitrosamines in total particulate matter in mainstream cig...
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
Inventor 唐纲岭陈晓水边照阳陈再根刘珊珊杨飞刘洋张洪非李中皓胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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