YC/T 184-2004 English PDF (YCT184-2004)

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YC/T 184-2004: Tobacco and tobacco products. Determination of tobacco specific N-nitrosamines
YC/T 184-2004
TOBACCO INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 65.160
X 87
Record number: 14402-2004
Tobacco and tobacco products -
Determination of tobacco specific N-nitrosamines
ISSUED ON: OCTOBER 19, 2004
IMPLEMENTED ON: MARCH 01, 2005
Issued by: State Tobacco Monopoly Administration
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Terms and definitions ... 4 
4 Principle ... 5 
5 Reagents ... 5 
6 Apparatus ... 6 
7 Analytical procedure ... 6 
8 Calculation of results ... 8 
9 Repeatability, recovery rate, and detection limit ... 8 
Appendix A (Informative) Examples of chromatograms ... 9 
Tobacco and tobacco products -
Determination of tobacco specific N-nitrosamines
1 Scope
This Standard specifies the method for determination of four tobacco specific
N-nitrosamines in tobacco and tobacco products [N-nitrosonornicotine (NNN),
N-nitrosanatabine (NAT), N-nitrosoanabasine (NAB), 4-(methylnitrosamine)-1-
(3-pyridyl)-1-butanone (NNK)].
This Standard applies to tobacco and tobacco products.
2 Normative references
The following documents contain provisions which, through reference in this
Standard, constitute provisions of this Standard. For the dated references, their
subsequent amendments (excluding corrections) or revisions do not apply to
this Standard. However, the parties who enter into agreement based on this
Standard are encouraged to investigate whether the latest editions of these
documents are applicable. For undated reference documents, the latest
editions apply to this Standard.
GB/T 5606.1 Cigarettes - Part 1: Sampling
GB/T 19616 Tobacco - Sampling of batches of raw material - General
principles (GB/T 19616-2004, ISO 4874:2000, MOD)
YC/T 31 Tobacco and tobacco products - Preparation of test sample and
determination of water content - Oven method
3 Terms and definitions
The following terms and definitions apply to this Standard.
3.1
Tobacco specific N-nitrosamines (TSNAs)
N-nitrosamines which exist only in tobacco and tobacco products.
Basic alumina (5.5) is activated at 110°C for 2 h for use. The chromatography
column (6.7) is kept clean and dry. First add 30 mL of methylene chloride (5.1);
ADD 15 g of basic alumina (5.5) after wet processing to the chromatography
column (6.7); USE a glass rod to stir the alumina to drive off bubbles. Then, add
2 g of dried anhydrous sodium sulfate; USE 50 mL of methylene chloride to
elute the chromatography column (6.7). When the liquid level drops to the
sodium sulfate layer, close the chromatography column piston.
7.4.2.2 Chromatography
ADD all the samples in the conical flask to the chromatography column (6.7);
USE 5 mL×3 of methylene chloride (5.1) to wash the inner wall of the conical
flask. The washing liquid is added to the chromatography column (6.7). After
the liquid level is close to the column head, use 30 mL of methylene chloride
(5.1) to elute the chromatography column (6.7). This part of the eluent is not
collected. Finally, use 100 mL of the solution with a methanol:methylene
chloride ratio of 8:92 (volume ratio) to elute the chromatography column (6.7);
COLLECT this part of eluent.
7.4.3 Concentration of eluent
Accurately add 100 μL of internal standard solution (5.6) to the eluent; under
high-purity nitrogen protection purge, concentrate it to about 1 mL; TRANSFER
it to a 2 mL chromatographic vial for GC-TEA analysis. Examples of
chromatograms of burley and flue-cured tobacco samples are given in
Appendix A.
7.5 GC-TEA analysis
7.5.1 Conditions of gas chromatograph (6.2)
7.5.1.1 Chromatographic column (6.3).
7.5.1.2 Pre-column guard column (6.4). It needs to be replaced after 100
sample analyses.
7.5.1.3 Temperature programming: The initial temperature is 50°C and
maintained for 2 min. At 10°C/min, rise it to 180°C and maintain for 10 min. At
10°C/min, rise it to 230°C. At 30°C/min, rise it to 260°C and maintain for 20 min.
7.5.1.4 Inlet temperature: 225°C.
7.5.1.5 Carrier gas: Helium, 2.5 mL/min.
7.5.1.6 Injection volume 2 μL, splitless. Splitless time is 1 min. Purge flow is 50
mL/min.