Vol. 35 No. 1 (2022): Revista ION
Articles

Development and evaluation of SPME-GC-MS method for the analysis of volatile organic compounds in cocoa liquor from Nariño- Colombia

Edna Jazmin Otero Rojas
Universidad de Nariño - Departamento de Quimica
Frank Carlos Herrera Ruales
Corporacion CIAD
David Arturo Perdomo
Corporacion CIAD
Juan Pablo Jimenez Mora
Corporacion CIAD

Published 2022-11-01

Keywords

  • Solid phase microextraction; chromatography; cocoa liquor; experimental design, fragrance

How to Cite

Otero Rojas, E. J., Herrera Ruales, F. C., Arturo Perdomo, D., & Jimenez Mora, J. P. (2022). Development and evaluation of SPME-GC-MS method for the analysis of volatile organic compounds in cocoa liquor from Nariño- Colombia. Revista ION, 35(1), 103–116. https://doi.org/10.18273/revion.v35n1-2022007

Abstract

In this research, the optimal conditions of time, temperature and fiber type were determined for the HS-SPME extraction method of volatile organic compounds (VOCs) presents in cocoa liquor, for this purpose, a factorial experimental design using the response surface methodology was applied. The optimal conditions determined in order to extract a greater number of VOCs through multivariable analysis were 50 min, 60 °C and the DVB/CAR-PDMS fiber. The precision of the method was adequate with a variation coefficient values (%CV) in terms of repeatability of 0.59 to 11.39 % and 4.29 to 12.93 % in reproducibility terms. The method development was carried out using a sample of cocoa liquor from CCN51 variety as reference, produced by the Cortepaz association in the municipality of Tumaco in Nariño-Colombia, according to the traditional fermentation, drying and roasting conditions implemented in the region. Using the optimal extraction conditions, 39 major VOCs were identified by gas chromatography coupled to mass spectrometry (GC- MS). The results determined that cocoa liquor mainly presented aldehyde, ketone, alcohol, pyrazine, ester, terpene, acid and lactone compounds, of which acetic acid, 2-propanol and 3-ethyl-2.5-dimethyl-pyrazine were found to the majority with a relative area percentages (%) of 46.16; 8.96 and 4.64 respectively.

Downloads

Download data is not yet available.

References

  1. Aprotosoaie AC, Luca SV, Myron A. Flavor Chemistry of Cocoa and Cocoa Products-An Overview. Compr. Rev. Food Sci. Food Saf. 2016;15(1):73-91. doi.org/10.1111/1541-4337.12180
  2. De Brito ES, Garcia NHP, Gallão M, Cortelazzo AL, Fevereiro PS, Braga MR. Structural and chemical changes in cocoa (Theobroma cacao L) during fermentation, drying and roasting. J. Sci. Food Agric. 2001;81:281-288. doi.org/10.1002/1097-0010(20010115)81:2<281::AID-JSFA808>3.0.CO;2-B
  3. Kongor JE, Hinneh M , De Walle D, Van Afoakwa EO, Boeckx P, Dewettinck K. Factors influencing quality variation in cocoa (Theobroma cacao) bean flavour profile - A review. Food Research International. 2016;82:44-52. doi.org/10.1016/j.foodres.2016.01.012
  4. Schwan R, Fleet G, Sarkar P, Nout MJR, Chen J, Zhu Y, Chandrasekaran M.Cocoa and Coffee Fermentations. Reino Unido:Taylor & Francis Group; 2015.
  5. Rodríguez J.Estudio de los compuestos volátiles de Theobroma cacao L., durante el proceso tradicional de fermentación, secado y tostado (Tesis doctoral). Ciudad de México, México. Instituto Politecnico Nacional. México; 2011.
  6. Rodriguez J, Escalona-Buendía HB, OrozcoAvila I, Lugo-Cervantes E, Jaramillo-Flores ME. Dynamics of volatile and non-volatile compounds in cocoa (Theobroma cacao L.) during fermentation and drying processes using principal components analysis. Food Research International. 2011;44(1):250-258. doi.org/10.1016/j.foodres.2010.10.028
  7. Ducki S, Miralles-Garcia J, Zumbe A, Tornero A, Storey DM. Evaluation of solid-phase microextraction coupled to gas chromatography–mass spectrometry for the headspace analysis of volatile compounds in cocoa products. Talanta. 2008;74:1166-1174. doi.org.10.1016/j.talanta.2007.08.034
  8. Pini GF, Brito ES, De García NHP, Valente ALP, Augusto, F. A Headspace Solid Phase Microextraction (HS-SPME) method for the chromatographic determination of alkylpyrazines in cocoa samples. J. Braz. Chem. Soc. 2004;15(2):267-271. doi.org/10.1590/S0103-50532004000200017
  9. Ziegleder G. Linalool contents as characteristic of some flavor grade cocoas. Z Lebensm Unters Forch.1990;191:306-309. doi.org/10.1007/BF01202432
  10. Jinap S, Thien J, Yap TN. Effect of drying on acidity and volatile fatty-acids content of cocoa beans. J. Sci. Food Agric. 1994;65(1):67-75. doi.org/10.1002/jsfa.2740650111
  11. Miralles-Garcia J. Chemical Composition and Flavour- Development of Cocoa Products by Thermal and Enzymatic Technologies (tesis doctoral). Manchester, England: University of Salford, A Greater Manchester University; 2008.
  12. Reineccius G. Flavor Chemistry and Technology. 2 ed. Estados Unidos: Taylor & Francis Group; 2006.
  13. Van Durme J, Ingels I, De Winne A. Inline roasting hyphenated with gas chromatography–mass spectrometry as an innovative approach for assessment of cocoa fermentation quality and aroma formation potential. Food Chem. 2016;205:66-72. doi.org/10.1016/j.foodchem.2016.03.004
  14. Rodríguez J, Escalona-Buendía HB, ContrerasRamos SM,Orozco-Avila I, Jaramillo-Flores E, Lugo-Cervantes E. Effect of fermentation time and drying temperature on volatile compounds in cocoa. Food Chem. 2012;132(1):277-288. doi.org/10.1016/j.foodchem.2011.10.078
  15. Qin X, Lai XW, Tan LH, Hao CY, Li FP , Hea SZ, Songa YH. Characterization of volatile compounds in Criollo, Forastero, and Trinitario cocoa seeds (Theobroma cacao L.) in China. Int. J. Food Prop. 2017;20(10):2261-2275. doi.org/10.1080/10942912.2016.1236270
  16. Tan J, Kerr WL. Determining degree of roasting in cocoa beans by artificial neural network (ANN)-based electronic nose system and gas chromatography/mass spectrometry (GC/MS). J. Sci. Food Agric. 2018;98(10):3851-3859. doi.org/10.1002/jsfa.8901
  17. Quijano CE, Pino J. Analysis of volatile compounds of cacao Maraco (Theobroma bicolor Humb. et Bonpl.) fruit. J. Essent. Oil Res. 2009;21(4):211-216. doi.org/10.1080/10412905.2009.9700150
  18. Di Carro M, Ardini F, Magi E. Multivariate optimization of headspace solidphase microextraction followed by gas chromatography-mass spectrometry for the determination of methylpyrazines in cocoa liquors. Microchem. J. 2015;121:172-177. doi.org/10.1016/j.microc.2015.03.006
  19. Counet C, Ouwerx C, Rosoux D, Collin S. Relationship between Procyanidin and Flavor Contents of Cocoa Liquors from Different Origins. J. Agric. Food Chem. 2004;52:6243-6249. doi.org/10.1021/jf040105b
  20. Kadow D, Bohlmann J, Phillips W, Lieberei R. Identification of main fine or flavour components in two genotypes of the cocoa tree (Theobroma cacao L.). J. Appl. Bot. Food Qual. 2013;86:90-98. doi.org/10.5073/JABFQ.2013.086.013
  21. Bastidas A. Estudio Químico de los Componentes Volátiles (HS-SPME) y Análisis de la Composición de Taninos y Cafeína en un Tipo de Café Tostado y Molido Tradicional Colombiano (Tesis de pregrado). Pasto, Colombia: Universidad de Nariño; 2011.
  22. Rojas-Monroy G. Caracterización del aroma del café molido de Puerto Rico mediante la técnica de microextracción; en fase sólida (SPME) y cromatografía de gas acoplada a espectrometría de masas GC/MS (Tesis de maestría). San Juan, Puerto Rico: Universidad de Puerto Rico; 2005.
  23. Balasubramanian S, Panigrahi S. Solid-Phase Microextraction (SPME) Techniques for Quality Characterization of Food Products: A Review. Food Bioprocess Technol. 2011;4(1):1-26. doi.org/10.1007/s11947-009-0299-3
  24. Menezes Filho A, Dos Santos FN, De Paula Pereira PA. Development, validation and application of a methodology based on solid-phase micro extraction followed by gas chromatography coupled to mass spectrometry (SPME/GC-MS) for the determination of pesticide residues in mangoes. Talanta. 2010;81(1-2):346-354. doi.org/10.1016/j.talanta.2009.12.008
  25. Ho VTT, Zhao J, Fleet G. Yeasts are essential for cocoa bean fermentation. Int. J. Food Microbiol. 2014;174:72-87. doi.org/10.1016/j.ijfoodmicro.2013.12.014
  26. Granda F, Valencia S, Marin JM, Restrepo G. Optimización del método de microextracción en fase sólida acoplada a cromatografía gaseosa para análisis de metanol en agua. Rev. Colomb. Quim. 2011;40(2):201-210.
  27. TGSC Information System. Características organolépticas. Base de datos en línea. (sitio de internet). Disponible en: http://www.thegoodscentscompany.com/data/rw1028161.html. Acceso el 1 de agosto de 2016.
  28. Afoakwa EO. Chocolate Science and Technology. 2 ed. Reino Unido: John Wiley & Son; 2016.
  29. Afoakwa EO, Paterson A, Fowler M, Ryan A. Flavor formation and character in cocoa and chocolate: A critical review. Crit. Rev. Food Sci. Nutr. 2008;48(9):840-857. doi.org/10.1080/10408390701719272
  30. Portillo E, Labarca M, Grazziani L, Cros E, Assemat S, Davrieux F, Boulanger R, Marcano M. Formación del aroma del cacao Criollo (Theobroma cacao L.) en función del tratamiento poscosecha en Venezuela. Revista Científica UDO Agricola. 2009;9(2):458-468.
  31. Frauendorfer F, Schieberle P. Changes in key aroma compounds of criollo cocoa beans durin groastin. J. Agric. Food Chem. 2008;56:10244-10251. doi.org/10.1021/jf802098f