YC/T 246-2008 English PDF (YCT246-2008)

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YC/T 246-2008: Tobacco and tobacco products. Determination of nicotine. Gas chromatographic method
YC/T 246-2008
TOBACCO INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 65.160
X 87
Record number: 23585-2008
Tobacco and tobacco products - Determination of
nicotine - Gas chromatographic method
ISSUED ON: APRIL 14, 2008
IMPLEMENTED ON: APRIL 14, 2008
Issued by: China Tobacco
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle ... 4 
4 Reagents and materials ... 4 
5 Instruments ... 6 
6 Analysis steps ... 6 
7 Calculation and expression of results ... 8 
8 Recovery and detection limit ... 8 
9 Test report ... 8 
Appendix A (Informative) Example of chromatogram ... 9 
Tobacco and tobacco products - Determination of
nicotine - Gas chromatographic method
1 Scope
This Standard specifies the gas chromatographic method for determination of
nicotine in tobacco and tobacco products.
This Standard applies to the determination of nicotine in tobacco and tobacco
products.
This Standard applies to samples whose nicotine content is 8 mg/g ~ 41 mg/g
(dry basis).
2 Normative references
The terms in the following documents become the terms of this Standard by
reference to this Standard. For dated references, all subsequent amendments
(not including errata content) or revisions do not apply to this standard. However,
parties to agreements that are based on this Standard are encouraged to study
whether the latest versions of these documents can be used. For undated
references, the latest edition applies to this Standard.
GB/T 5606.1, Cigarettes - 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 Principle
Use an organic solvent to extract the nicotine in the sample; use a gas
chromatograph that is equipped with a flame ionization detector to perform the
determination; use the internal standard method to quantify.
4 Reagents and materials
4.1 Except for special requirements, analytical reagents shall be used.
flasks respectively; use the extraction solution (4.12) to dilute the volume to the
mark, to obtain different concentrations of nicotine working standard solutions;
the concentration range shall cover the concentration of nicotine that is
expected to be detected in the sample.
5 Instruments
5.1 Volumetric flasks, 50 mL, 100 mL, 250 mL.
5.2 Triangular flasks, 100 mL, 250 mL, with stopper.
5.3 Oscillator.
5.4 Gas chromatograph: it is equipped with a flame ionization detector.
6 Analysis steps
6.1 Sampling
Cigarette samples are sampled according to GB/T 5606.1.
Tobacco leaf samples are sampled according to GB/T 19616.
6.2 Sample preparation
Prepare samples and measure the moisture content according to YC/T 31.
6.3 Extraction
6.3.1 Methyl-tert-butyl ether method
Accurately weigh (1.000 ± 0.020) g of sample in a triangular flask (5.2); use a
10 mL polytetrafluoroethylene pipette to transfer 7 mL of sodium hydroxide
solution (4.5) into the extraction bottle; gently shake the extraction bottle; wet
test sample; let stand for 15 min. Then, add 50 mL of extraction solution (4.11);
seal with lid and place on the oscillator (5.3); shake and extract for 2 h. Let
stand to separate the sample from the extractant (up to 24 h); take the
supernatant for analysis.
6.3.2 N-hexane method
Accurately weigh 1 g ~ 2 g of sample, accurate to 0.001 g; put it in a 100 mL
triangular flask (5.2); add 20 mL of water, 40 mL of extraction solution (4.12)
and 10 mL of sodium hydroxide solution (4.6); put it on the oscillator (5.3); shake
and extract for 60 min. After standing, take the upper organic phase and
immediately analyze by gas chromatography. The extraction bottle can also be
placed in an ultrasonic water bath to facilitate the separation of the two phases.
6.4 Determination
6.4.1 Instrument preparation
Set up and operate the gas chromatograph (5.4) according to the operating
instructions. Ensure that the solvent peak, internal standard peak, and nicotine
peak are completely separated. The analysis conditions of the following gas
chromatograph can be used for reference; the applicability of other conditions,
if adopted, shall be verified.
See Appendix A for the chromatogram of the sample extract.
6.4.2 Chromatographic conditions (methyl-tert-butyl ether method)
Chromatographic column: a capillary column whose column length is 30 m and
inner diameter is 0.32 mm or 0.25 mm; stationary phase: 5% phenyl-methyl
polysiloxane.
Carrier gas: helium; inlet temperature: 250 °C; detector temperature: 250 °C;
sampling method: split sampling; split ratio: 40:1; injection volume: 1.0 μL;
column flow rate: 1.7 mL/min.
Adopt temperature programming method:
-- Initial temperature: 110 °C; initial time: 0 min;
-- Temperature programming 1: increase from 110 °C to 185 °C at a rate of
10 °C/min;
-- Temperature programming 2: increase from 185 °C to 245 °C at a rate of
6 °C/min; keep for 10 min;
-- Total running time: 27.5 min.
6.4.3 Chromatographic conditions (n-hexane method)
Chromatographic column: a capillary column whose column length is 15 m and
inner diameter is 0.53 mm; stationary phase: 50% phenyl-methyl polysiloxane.
Carrier gas: helium or hydrogen; inlet temperature: 270 °C; detector
temperature: 270 °C; sampling method: split sampling; split ratio: 10:1; injection
volume: 1.0 μL; column flow rate: 7 mL/min;
Adopt isothermal mode; column temperature: 170 °C; total running time: 10 min.
6.4.4 Preparation of the standard curve