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Development and Validation of 2D GC-FID Method for Quantitative Analysis of cis- and trans-Hexyl Cinnamic Aldehyde and its Major Impurity 2-Hexyl-2-decenal
Corresponding Author(s) : Rahul V. Pinjari
Asian Journal of Chemistry,
Vol. 30 No. 5 (2018): Vol 30 Issue 5, 2018
Abstract
Hexyl cinnamic aldehyde (HCA) is an aroma chemical used as a flavour and fragrance ingredient, which is synthesized in huge quantity worldwide. The hexyl cinnamic aldehyde present in the trans- and cis-forms with nearly 95:5 ratio. The 2-hexyl-dec-2-enal (HDEA) is process impurity in hexyl cinnamic aldehyde, which may amount upto ~ 2.0 %. However use of 2-hexyl-dec-2-enal is prohibited in the fragrance, while in flavours the Flavour and Extract Manufacturer Association (FEMA) has permitted its concentration only up to 5.0 ppm. Thus a simple and rapid two dimensional gas chromatographic method (2D-GC) for quantitative analysis of (cis-/trans-)hexyl cinnamic aldehyde and 2-hexyl-dec-2-enal have been developed. The non-polar and polar capillary columns are connected in series and the flame ionization detector with nitrogen carrier is used. The method yields a well separated cis-hexyl cinnamic aldehyde, trans-hexyl cinnamic aldehyde and 2-hexyl-dec-2-enal peaks from the other impurities. The method is validated according to the ICH guideline for precision, recovery, linearity, and limit of detection.
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References
T. Rustemeyer, P. Elsner, S.M. John and H.I Maibach, Kanerva's Occupational Dermatology, Aromatherapist, 118, 1266 (2012).
(a) G. Shi-long, China Surf. Det. Cosm. Syn., 1, 17 (2006); (b) Z. Lirong and Y. Feng-ping, Chem. World, 12, 10 (2014).
International Fragrance Association (IFRA); α-Hexyl Cinnamic aldehyde, 47th amendment (2013).
S.M. Cohen, S. Fukushima, N.J. Gooderham, S.S. Hecht, L.J. Marnett, I.M.C.M. Rietjens, R.L. Smith, M. Bastaki, M.M. Mcgowen, C. Harman and S.V. Taylor, 27th publication by the Expert Panel of Flavor and Extract Manufacturers. Association (FEMA), GRAS 27, Food Technology (2011).
D. Rowe, Chemistry and Technology of Flavor and Fragrances, WileyBlackwell Publishing Ltd, UK, edn 1, p. 351 (2009).
Sigma-Aldhrich, GC Column Selection Guide, Achieve Optimal Method Performance, Nicholas, Walter, p. 22.
C. Vendeuvre, R. Ruiz-Guerrero, F. Bertoncini, L. Duval and D. Thiébaut, Oil Gas Sci. Technol., 62, 43 (2007); https://doi.org/10.2516/ogst:2007004.
V. Ravichandra, S. Shalini, K.M. Sundram and R. Harish, Int. J. Pharm. Pharm. Sci., 2(Suppl 3), 18 (2010).
Column Selection Principles, Agilent J&W GC Column Selection Guide, pp. 19.
A.G. Piantanida and A. R. Barron, Principles of Gas Chromatography, OpenStax-CNX, (1.2) pp. 1-12 (2014).
ICH Expert, ICH Harmonized Tripartite Guideline, Validation of Analytical Test Procedures and Method, Q2(R1), pp. 17 (2005).
J. Vessman, R.I. Stefan, J.F. van Staden, K. Danzer, W. Lindner, D.T. Burns, A. Fajgelj and H. Müller, Pure Appl. Chem., 73, 1381 (2001); https://doi.org/10.1351/pac200173081381.
S.B. Puranik, V.R. Pawar, N. Lalitha, P.N.S. Pai and G.K. Rao, Orient. J. Chem., 24, 529 (2008).