Rapid and Simple Extraction Method for Volatile N-Nitrosamines in Meat Products


A new methodology for extraction, pre-concentration and analysis of volatile nitrosamines in meat-derived products was developed and compared with conventional methods (Distillation and two-step solid-phase extraction). The samples (canned sausages, cured meat, luncheon and smoked meat) were treated with an aqueous sodium hydroxide (NaOH) by autoclaving at 121°C for 10 min and extracted by liquid-liquid extraction with dichloromethane, then the nitrosamines were pre-concentrated using activated silica. Then, gas chromatography coupled with flame ionization detector was used for the separation and determination of the different nitrosamines contained in a real sample and gas chromatography with mass spectrometry detection was used as the confirmation technique. The newly invented autoclaving method allowed the determination of nitrosamine compounds at trace levels with limit of detection ranged from 0.077 to 0.18 ppb and quantitation limits were from 0.26 to 0.6 ppb for all nitrosamines, and found to be superior to the conventional ones, yielding approximately about 10%-20% increasing in the recovery compared with the mean recovery obtained when applying conventional methods.

Share and Cite:

Al-Kaseem, M. , Al-Assaf, Z. and Karabet, F. (2013) Rapid and Simple Extraction Method for Volatile N-Nitrosamines in Meat Products. Pharmacology & Pharmacy, 4, 611-618. doi: 10.4236/pp.2013.48087.

Conflicts of Interest

The authors declare no conflicts of interest.


[1] M. W. Byun, H. J. Ahn, J. H. Kim, J. W. Lee, H. S. Yook and S. B. Han, “Determination of Volatile N-Nitrosamines in Irradiated Fermented Sausage by Gas Chromatography Coupled to a Thermal Energy Analyzer,” Journal of Chromatography A, Vol. 1054, No. 1-2, 2004, pp. 403-407.
[2] IARC Monographs on the Evaluation of Carcinogenic Risks to Humans, “Monographs Programme Finds Smokeless Tobacco Is Carcinogenic to Humans,” International Agency for Research on Cancer, 2004.
[3] D. Kocak, M. Z. Ozel, F. Gogus, J. F. Hamilton and A. C. Lewis, “Determination of Volatile Nitrosamines in Grilled Lamb and Vegetables Using Comprehensive Gas Chromatography—Nitrogen Chemiluminescence Detection,” Food Chemistry, Vol. 135, No. 4, 2012, pp. 2215-2220. http://dx.doi.org/10.1016/j.foodchem.2012.07.002
[4] N. Campillo, P. Vinas, N. C. Martinez and M. H. Córdoba, “Determination of Volatile Nitrosamines in Meat Products by Microwave-Assisted Extraction and Dispersive Liquid-Liquid Micro-Extraction Coupled to Gas Chromatography-Mass Spectrometry,” Journal of Chromatography A, Vol. 1218, No. 14, 2011, pp. 1815-1821.
[5] W. G. Lin, F. Wei, F. N. Gu, X. Dong, L. Gao, T. T. Zhuang, M. B. Yue and J.H. Zhu, “Adsorption of Nitrosamines by Mesoporous Zeolite,” Journal of Colloid and Interface Science, Vol. 348, No. 2, 2010, pp. 621-627.
[6] R. Andrade, F. G. Reyes and S. Rath, “A Method for the Determination of Volatile N-Nitrosamines in Food by HS-SPME-GC-TEA,” Food Chemistry, Vol. 91, No. 1, 2005, pp. 173-179.
[7] B. J. Sanchez, E. Ballesteros and M. Gallego, “Automatic Screening Method for the Pre-Concentration and Determination of N-Nitrosamines in Water,” Talanta, Vol. 73, No. 3, 2007, pp. 498-504.
[8] K. O. Honikel, “The Use and Control of Nitrate and Nitrite for the Processing of Meat Products,” Meat Science, Vol. 78, No. 1-2, 2008, pp. 68-76.
[9] R. A. Scanlan, “Encyclopedia of Food and Nutrition,” Elsevier, 2003, pp. 4142-4147.
[10] M. J. Dennis, P. E. Key, T. Papworth, M. Pointer and R. C. Massey, “The Determination of Nitrate and Nitrite in Cured Meat by HPLC/UV,” Food Additives and Contaminants, Vol. 7, No. 4, 1990, pp. 455-461.
[11] F. E. Okieimana, E. O. Akintola, T. C. A. Anucha and M. M. Ajibola, “Determination of Total Level of Nitrosamine Contamination of Some Consumer Products in Nigeria,” International Journal of Environmental Analytical Chemistry, Vol. 21, No. 4, 1985, pp. 261-266.
[12] M. T. Matyska, J. J. Pesek and L. Yang, “Screening method for Determining the Presence of N-Nitrosodiethanolamine in Cosmetics by Open-Tubular Capillary Electrochromatography,” Journal of Chromatography A, Vol. 887, No. 1-2, 2000, pp. 487-503.
[13] M. Qiang, X. H. Wei, W. Chao, B. Hua, X. G. Cheng, S. Ning, X. L. Yan and W. J. Bing, “Determination of Ten Volatile Nitrosamines in Cosmetics by Gas Chromatography Tandem Mass Spectrometry,” Chinese Journal of Analytical Chemistry, Vol. 39, No. 8, 2011, pp. 1201-1207. http://dx.doi.org/10.1016/S1872-2040(10)60466-5
[14] J. E. Grebel and H. I. Suffet, “Nitrogen-Phosphorus Detection and Nitrogen Chemiluminescence Detection of Volatile Nitrosamines in Water Matrices: Optimization and Performance Comparison,” Journal of Chromatography A, Vol. 1175, No. 1, 2007, pp. 141-144.
[15] M. Z. Ozel, F. Gongus, S. Yagci, J. F. Hamilton and A. C. Lewis, “Determination of Volatile Nitrosamines in Various Meat Products Using Comprehensive Gas Chromatography-Nitrogen Chemiluminescence Detection,” Food and Chemical Toxicology, Vol. 48, No. 11, 2010, pp. 3268-3273. http://dx.doi.org/10.1016/j.fct.2010.08.036
[16] B. Hfiger and R. Niessner, “Determination of N-Nitrosomethylaniline and Methylaniline in the Gas Phase,” Microchimica Acta, Vol. 122, No. 1-2, 1996, pp. 35-44.
[17] J. A. Incavo and M. A. Schafer, “Simplified Method for the Determination of N-Nitrosamines in Rubber Vulcanizates,” Analytica Chimica Acta, Vol. 557, No. 1-2, 2006, pp. 256-261. http://dx.doi.org/10.1016/j.aca.2005.10.018
[18] D. Tsikas, “Methods of Quantitative Analysis of the Nitric Oxide Metabolites Nitrite and Nitrate in Human Biological Fluids,” Free Radical Research, Vol. 39, No. 8, 2005, pp. 797-815.
[19] J. W. Dallinga, D. M. Pachen, A. H. Lousberg, J. A. Van Geel, G. M. Houben, R. W. Stockburgger, J. M. Maanen and J. C. Kleinjans, “Volatile N-Nitrosamines in Gastric Juice of Patients with Various Conditions of the Gastrointestinal Tract Determined by Gas Chromatography-Mass Spectrometry and Related to Intragastic pH and Nitrate and Nitrite Levels,” Cancer Letters, Vol. 124, No. 2, 1998, pp. 119-125.
[20] Y. Xia, J. E. McGuffey, S. Bhattacharyya, B. Sellergren, E. Yilmaz and L. Wang, “Analysis of the Tobacco-Specific Nitrosamine 4-(Methylnitrosamino)-1-(3-Pyridyl)-1-Butanol in Urine by Extraction on a Molecularly Imprinted Polymer Column and Liquid Chromatography/ Atmospheric Pressure Ionization Tandem Mass Spectrometry,” Analytical Chemistry, Vol. 77, No. 23, 2005, pp. 7639-7645. http://dx.doi.org/10.1021/ac058027u
[21] G. Bellec, M. C. Cauvin, K. L. Calve, Y. Dreano, H. Gouerou, J. F. Menez and F. Berthou, “Analysis of N-Nitrosamines by High-Performance Liquid Chromatography with Post-Column Photohydrolysis and Colorimetric Detection,” Journal of Chromatography A, Vol. 727, No. 1, 1996, pp. 83-92.
[22] N. V. Komarova and A. A. Velikanov, “Determination of Volatile N-Nitrosamines in Food by High-Performance Liquid Chromatography with Fluorescence Detection,” Journal of Analytical Chemistry, Vol. 56, No. 4, 2001, pp. 359-363. http://dx.doi.org/10.1023/A:1016652213062
[23] Association of Official Analytical Chemists, “N-Nitrosamines (Volatile) in Fried Bacon. Mineral Oil Vacuum Distillation—Thermal Energy Analyzer Method,” No. 982.22, Official Methods of Analysis, 15th Edition, 1990.
[24] E. L. Greenfield, W. J. Smith and A. J. Malanovski, “Mineral Oil Vacuum Distillation for Nitrosamines in Fried Bacon, with Thermal Energy Analyser,” Journal of the Association Official Analytical Chemists, Vol. 65, No. 6, 1982, pp. 1319-1332.
[25] G. M. Telling, T. A. Bryce and J. J. Althorpe, “Use of Vacuum Distillation and Gas Chromatography-Mass Spectrometry for Determining Low Levels of Volatile Nitrosamines in Meat Products,” Journal of Agricultural and Food Chemistry, Vol. 19, No. 5, 1971, pp. 937-940.
[26] J. Nawrocki and P. Andrzejewski, “Nitrosamines and Water,” Journal of Hazardous Materials, Vol. 189, No. 1-2, 2011, pp. 1-18.
[27] S. Raoul, E. Gremaud, H. Biaudet and R. Tureski, “Rapid Solid-Phase Extraction Method for the Detection of Volatile Nitrosoamines in Food,” Journal of Agricultural and Food Chemistry, Vol. 45, No. 12, 1997, pp. 4706-4713.
[28] S. Ventanas, D. Martín, M. Estévez and J. Ruiz, “Analysis of Volatile Nitrosamines from a Model System Using SPME-DED at Different Temperatures and Times of Extraction,” Food Chemistry, Vol. 99, No. 4, 2006, pp. 842-850. http://dx.doi.org/10.1016/j.foodchem.2005.08.035
[29] W. Fiddler and J. W. Pensabene, “Supercritical Fluid Extraction of Volatile N-Nitrosamines in Fried Bacon and Its Drippings: Method Comparison,” Journal of AOAC International, Vol. 79, No. 4, 1996, pp. 895-901.
[30] International Conference on Harmonization, “Validation of Analytical Procedure, Text and Methodology Q2 (R1),” 2005 IFPMA, Geneva, Switzerland.
[31] M. L. Nollet and F. Toldra, “Handbook of Processed Meats and Poultry Analysis,” In: S. Rath and F. G. R. Reyes, Nitrosamines, Taylor & Francis Group, An Informa Business, New York, 2009, p. 688.
[32] S. Yurchenko and U. Molder, “The Occurrence of Volatile N-Nitrosamines in Estonian Meat Products,” Food Chemistry, Vol. 100, No. 4, 2007, pp. 1713-1721.

Copyright © 2024 by authors and Scientific Research Publishing Inc.

Creative Commons License

This work and the related PDF file are licensed under a Creative Commons Attribution 4.0 International License.