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YC/T 184-2004 PDF English

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YC/T 184-2004: Tobacco and tobacco products. Determination of tobacco specific N-nitrosamines
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GB 5606.2   GB/T 5606.1   YC/T 605   

YC/T 184-2004: Tobacco and tobacco products. Determination of tobacco specific N-nitrosamines

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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. ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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