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Classification of Coffee Beans by GC-C-IRMS, GC-MS, and H-NMR

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Classification of Coffee Beans by GC-C-IRMS, GC-MS, and H-NMR Hindawi Publishing Corporation Journal of Analytical Methods in Chemistry Volume 2016, Article ID 8564584, 11 pages http://dx.doi.org/10.1155/2016/8564584 Research Article Classification of Coffee Beans by GC-C-IRMS, 1 GC-MS, and H-NMR Victoria Andrea Arana,1 Jessica Medina,2 Pierre Esseiva,3 Diego Pazos,3 and Julien Wist2 1 Grupo de Investigacion´ Ciencias, Educacion´ y Tecnolog´ıa (CETIC), Programa de Qu´ımica, Facultad de Ciencias Basicas,´ Universidad del Atlantico,´ km 7 Antigua V´ıa Puerto Colombia, Barranquilla, Atlantico,´ Colombia 2Chemistry Department, Universidad del Valle, A.A. 25360, Cali, Colombia 3Institut de Police Scientifique, Ecole´ des Sciences Criminelles, UniversitedeLausanne,1015Lausanne,Switzerland´ Correspondence should be addressed to Julien Wist; [email protected] Received 1 April 2016; Accepted 15 June 2016 Academic Editor: Karoly Heberger Copyright © 2016 Victoria Andrea Arana et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. 1 In a previous work using H-NMR we reported encouraging steps towards the construction of a robust expert system for the discrimination of coffees from Colombia versus nearby countries (Brazil and Peru), to assist the recent protected geographical indication granted to Colombian coffee in 2007. This system relies on fingerprints acquired on a 400 MHz magnet and is thus well suited for small scale random screening of samples obtained at resellersorcoffeeshops.However,thisapproachcannoteasilybe implemented at harbour’s installations, due to the elevated operational costs of cryogenic magnets. This limitation implies shipping the samples to the NMR laboratory, making the overall approach slower and thereby more expensive and less attractive for large scale screening at harbours. In this work, we report on our attempt to obtain comparable classification results using alternative techniques that have been reported promising as an alternative to NMR: GC-MS and GC-C-IRMS. Although statistically significant information could be obtained by all three methods, the results show that the quality of the classifiers depends mainly on the number of variables included in the analysis; hence NMR provides an advantage since more molecules are detected to obtain a model with better predictions. 1. Introduction hasbeenusedasmarkersforenvironmentalconditionsand agricultural practices, as well as for the identification of the Colombian coffee is a protected geographical indication origin of coffee [1, 2]. Using the same technique, Rodrigues et (PGI), a recognition for its high quality, and the result of al. [3] determined that the differences in geographic location decades of efforts and strategies to federate more than half are due mainly to altitude and precipitation. Near-Infrared a million coffee growers. Moreover, the consumption of high Spectroscopy (NIRS), Mass Spectrometry (MS), and Nuclear profile coffees from specific origins is constantly increasing, Magnetic Resonance (NMR) have initially been applied to meaning that the 100% Colombian coffee label represents an determine the composition of mixtures of Coffea arabica L. economical plus-value for local growers. In addition, Colom- and Coffea canephora var. robusta [4–13], before targeting bia imports coffee from neighboring countries to supply its the determination of the origin of coffee beans. Hyphenated internal market. This context calls for methods able to ensure separation methods coupled to Mass Spectrometry, such the quality and origin of the coffee beans. Ideally, they should as HS-SPME-GC-TOF-MS for the detection of volatile and be sufficiently robust and cost-effective to be implemented at semivolatile compounds and LC-MS and GC-FID for the harbour installations for screening of material immediately quantification of amino acids and carbohydrates, could also after arrival or just before being shipped. distinguish coffees from different origin [14, 15]. Several efforts have been directed to this aim; the stable A very nice review by Kelly et al. [16] lists the different 2 13 15 18 isotopes composition, such as H, C, N, and O, techniques that have been successfully applied to the deter- determined by Isotope Ratio Mass Spectrometry (IRMS) mination of origin of food products, while an up-to-date list 2 Journal of Analytical Methods in Chemistry of articles that report on the determination of origin of coffee oneproposedbyWeckerleetal.[19]andstartswitha canbefoundinTable1.Atfirstglance,itcanbeappreciated liquid-liquid extraction. First, 80 mg of coffee powder was that a wide range of methods have been evaluated and second extracted in 1 mL of boiling water during 10 min agitation by that only a small fraction of contributions are based on vortex. The filtered solution was subjected to liquid-liquid NMR. More interestingly, looking at the sampling schemes extraction with 1 mL of chloroform during 10 min vortex. reported, in particular the choice of countries per continents, The organic phase was dried over anhydrous Na2SO4 and indicates that these results should be considered with care filtered. Subsequently, 180 L of extract was transferred to a and that further evaluations are required to evidence the vial and 20 L of tetradecanoic acid methyl ester (40 g/mL) potential of such methods for precise localization of samples, was added as internal standard. For GC-MS samples, 200 mg for example, to distinguish between neighboring countries. of finely ground coffee was extracted at room temperature In addition, the sources of variance that may influence the in 1 mL of dichloromethane. After two-minute agitation with profiles in one country, altitude, precipitations, postharvest vortex, the samples were filtered and transferred to a vial 1 processing, and so forth, are hardly accounted for in such with 0.2 mg/mL of 1-decanol as internal standard. For H- experimental design. Last but not least, another important NMR, 200 mg of finely ground coffee powder was extracted at issueisuncoveredfromTable1:mostcontributionsreport room temperature in 1 mL HPLC grade methanol. After two- on a single technique making comparison between them very minute agitation with vortex, the samples were centrifuged ∘ impractical. for 10 min at 17 Cand450L of the extract was transferred 1 Inapreviouswork[17]wehaveshownthat H-NMR led to the NMR tube. Last, 90 L of deuterated methanol with to accurate discrimination of roasted Colombian beans when TMS was added. usingsamplescollectedduringseveralyearsandfromallover Colombia forming, in a good approximation, a representative 2.2. Analytical Techniques set of Colombian coffees. In addition, a large set of samples 13 fromthesameperiodoftimeandcollectedfromallover 2.2.1. GC-C-IRMS. The C values of caffeine were deter- the world formed the best possible approximation to a repre- mined with a Delta V Advantage Isotope Ratio Mass Spec- sentative set of non-Colombian samples. In this contribution trometer (IRMS) system (Thermo Fisher Scientific, Bremen, a subset of these collections was carefully chosen to retain Germany) coupled to a Trace GC Ultra Gas Chromatograph most of the sources of variance and was analyzed using two via a GC-C/TC III interface operating in the “Combustion” additional methods as an attempt to obtain a fair comparison (C) mode and equipped with a TriPlus6 autosampler. DB- 17MS GC column was used for the separation with the fol- of their abilities to distinguish coffees from Colombia, Peru, ∘ lowing operating conditions: injection temperature, 280 C; and Brazil. In Section 2 we will describe the sample set, ∘ ∘ oven temperature, 70 Cfor2min,rampat15C/min to reach the preparation protocols, and the chemometrics methods. ∘ ∘ ∘ In Section 3 we present our results. Finally, conclusions are 160 C, ramp at 10 C/min up to 280 C, and constant temper- provided in Section 4. aturefor2min.Thetotalrundurationwasof32minutes. A constant flow (1.6 mL/min) of helium gas was injected as carrier gas and 1 L of sample solution was injected in splitless 2. Materials and Methods mode. The detection of ions at 44, 45, and 46 m/z is carried outbyanimpactsourcewitha3kVaccelerationvoltage,a 2.1. Samples Collection and Preparation. A total of 34 samples magnetic field, and a Faraday collector for the measurement of each mass. The temperatures inside the combustion and of roasted coffees (Coffea arabica L.) were collected over a ∘ ∘ two-year period, 2012 to 2013, from 3 different countries reduction ovens were of 940 Cand600C, respectively. Six of South America. The samples were provided by Almacafe´ pulses of reference gas, CO2,of20seachwereintroduced S.A. (Colombia) and distributed as follows: 15 samples from during the chromatographic separation. Complete oxidation Colombia, 11 from Brazil, and 8 from Peru. Colombian coffee of the combustion chamber was performed after each batch samples were distributed as follows: 2 samples came from of 20 samples. Randomly chosen duplicates were intertwined coffee farms located in the Department of Tolima, 4 samples between runs to check for experimental error. Acquisition came from Huila, and 9 samples came from Narino.˜ Each and evaluation of GC-C-IRMS data were performed with delivered parcel contained samples from different origins software ISODAT 2.5 (Thermo Fisher Scientific, Bremen, Germany). After the complete conversion of the C atoms into according to harvests. ∘ It is important
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