Effect of Roasting Level on the Development of Key Aroma-Active Compounds in Coffee.

Coffee roasting is considered the most critical process in the development of sensory characteristics. During this stage, a substantial number of compounds are generated. Nevertheless, only a limited number of these compounds are responsible for the aroma, referred to as key aroma-active compounds. This study aimed to assess the impact of roasting levels on the formation of these compounds. Coffee was roasted at four different levels: very light (RL85), light (RL75), medium (RL55), and extremely dark (RL25), according to the Specialty Coffee Association (SCA) guidelines. The extraction, olfactory evaluation, and identification of compounds were performed using solid-phase microextraction (SPME), gas chromatography-olfactometry (GC-O), and gas chromatography-mass spectrometry (GC-MS), respectively. A total of 74 compounds were successfully identified, of which 25 were classified as aroma-active compounds. RL75 and RL85 displayed similar aromatic profiles. RL55 was characterized by pleasant notes such as sweet, toasted hazelnut, and caramel. In contrast, RL25 was marked by undesirable odors including burnt notes, putrid, and sulfurous scents. This study is the first to identify key odorant compounds in coffee based on SCA roasting standards.

Coffee Oil Extraction Methods: A Review.

Green and roasted coffee oils are products rich in bioactive compounds, such as linoleic acid and the diterpenes cafestol and kahweol, being a potential ingredient for food and cosmetic industries. An overview of oil extraction techniques most applied for coffee beans and their influence on the oil composition is presented. Both green and roasted coffee oil extractions are highlighted. Pressing, Soxhlet, microwave, and supercritical fluid extraction were the most used techniques used for coffee oil extraction. Conventional Soxhlet is most used on a lab scale, while pressing is most used in industry. Supercritical fluid extraction has also been evaluated mainly due to the environmental approach. One of the highlighted activities in Brazilian agribusiness is the industrialization of oils due to their increasing use in the formulation of cosmetics, pharmaceuticals, and foods. Green coffee oil (raw bean) has desirable bioactive compounds, increasing the interest of private companies and research institutions in its extraction process to preserve the properties contained in the oils.

Integrated effect of yeast inoculation and roasting process conditions on the neo formed contaminants and bioactive compounds of Colombian roasted coffee (Coffea arábica).

The rational design of methodologies to control the neoformed compounds occurrence (NFCs), such as acrylamide and hydroxymethylfurfural (HMF) in roasted coffee, must consider the preservation of the bioactive compounds contained in this beverage. The aim of this work was to evaluate the integrated effect of yeast inoculation during the fermentation stage and the modification of roasting parameters on the final concentrations of NFCs and bioactive compounds of roasted coffee. A completely randomized factorial design was used to evaluate the effect of yeast inoculation (with and without inoculation), roasting temperature (150, 180 and 210 °C) and roast degree (medium, dark) on the (i) physicochemical characteristics (volume change, mass loss, water activity, non-enzymatic browning index, antioxidant capacity, total polyphenols, chlorogenic acid and caffeine) as well as HMF and acrylamide levels of roasted coffee. Response variables were analyzed separately by ANOVA and clustering of treatments was explored by PCA. Yeast inoculation did not significantly (p > 0.05) affect volume change, mass loss, antioxidant capacity, total polyphenols content, and caffeine contents. The interaction of evaluated factors significantly decreased (p < 0.05) the acrylamide and HMF contents of roasted coffee (43 % and 56.0 %, respectively). Based on PCA grouping the best treatments were medium roast at 210 °C (inoculated and uninoculated) and at 180 °C (inoculated). Under these conditions it is possible to produce a roasted coffee mitigated in neo formed contaminants that present the physicochemical properties of original product.

Determination of ochratoxin A in coffee by ELISA method and its relationship with the physical, physicochemical and microbiological properties / Determinación de ocratoxina A en café mediante método ELISA y su relación con las propiedades físicas, fisicoquímicas y microbiológicas

Background: Coffee is one of the most consumed beverages in the world; however, it may contain toxic compounds such as ochratoxin A (OTA). Objectives: Determine the OTA's presence in different types of coffee, intended for beverage preparation and marketed in Colombia through the application of the enzyme-linked immunosorbent assay (ELISA) and analyze its relationship with the physical, physicochemical and microbiological properties. Methods: 8 samples of coffee commercialized in the Colombian market were selected, in which the OTA content was determined by applying the ELISA method. Likewise, a microbiological analysis was performed, and physicochemical properties were determined, such as moisture content, aw, percentage total dissolved solids (%TDS), and extraction yield (%EY). Physical properties such as free-flow densities, compacted bulk densities (CBD), porosity, average particle size (ASP), and color. The data were treated with multivariate analysis using Principal Component Analysis (PCA) and Cluster Analysis (CA) to quantitatively investigate the relationships between the coffee samples concerning their physical, physicochemical properties, and OTA content. LSD test was applied with a significance level of 95 % and Pearson correlation test. Results:All the samples had OTA content, but only 2 exceeded the limits allowed by the regulations, with a maximum value of 15.449 µg/Kg, which represents 31.449 % of the tolerable daily intake according to the parameters defined by Joint FAO/WHO Expert Committee on Food Additives (JECFA). According to the PCA and CA, the samples were grouped harmonically according to the type of coffee associated with its commercial presentation and industrial process, OTA content, and ASP. OTA content was significantly and positively correlated (p< 0.05) with %EY, %TDS, ASP, porosity, CBD and moisture. Conclusions: The coffees marketed in Colombia showed a variable range of OTA, where soluble coffees had higher OTA contents than roasted coffees, and 25 % of the coffees analyzed do not meet the levels defined by Colombian regulations. The OTA content in coffee is related to properties that define the ability to extract solutes from coffee

Antecedentes: El café es una de las bebidas más consumidas en el mundo, sin embargo, puede contener compuestos tóxicos como la ocratoxina A (OTA). Objetivos: Determinar la presencia de OTA en diferentes tipos de café destinados a la preparación de bebida y comercializados en Colombia mediante la aplicación del ensayo inmunoabsorbente ligado a enzimas (ELISA) y analizar su relación con las propiedades físicas, fisicoquímicas y microbiológicas. Métodos: Se seleccionaron 8 muestras de café comercializado en el mercado colombiano, en las cuales se determinó el contenido de OTA mediante la aplicación del método ELISA. Así mismo se realizó análisis microbiológico y se determinaron propiedades fisicoquímicas como contenido de humedad, aw, porcentaje de sólidos disueltos totales (%TDS) y rendimiento de extracción (%EY); y propiedades físicas como densidad por caída libre, densidad compactada (CBD), porosidad, tamaño promedio de partícula (ASP) y color. Los datos fueron tratados con análisis multivariado empleando análisis de componentes principales (PCA) y análisis de conglomerados (CA) para investigar cuantitativamente las relaciones entre las muestras de café con respecto a sus propiedades físicas, fisicoquímicas y contenido de OTA. Se aplicó prueba LSD con un nivel de significación del 95 % y prueba de correlación de Pearson. Resultados: Todas las muestras presentaron contenido de OTA, pero solo 2 sobrepasaron los límites permitidos por la normatividad, con un valor máximo de 15.449 µg/Kg, el cual representa un 31.449 % de la ingesta diaria tolerable según los parámetros definidos por el Comité Mixto FAO/OMS de Expertos en Aditivos Alimentarios (JECFA). De acuerdo al PCA y CA, las muestras se agruparon armónicamente de acuerdo al tipo de café asociado a su presentación comercial y proceso industrial, contenido de OTA y ASP; el contenido de OTA se correlacionó significativa y positivamente (p < 0.05) con el %EY, %TDS, ASP, porosidad, CBD y humedad. Conclusión: Los cafés comercializados en Colombia presentan un rango variable de OTA, en donde los cafés solubles presentan contenidos de OTA mayores que los cafés tostados y el 25 % de los cafés analizados no cumplen con niveles definidos por la normatividad colombiana. El contenido de OTA en el café está relacionado con propiedades que definen la capacidad de extracción de solutos del café

Characterization of Roasted Coffea arabica Species by the Relationship Between Caffeine and Diterpenes Contents

Abstract Commercial roasted and ground coffees are usually blends of Coffea arabica and Coffea canephora. Considering the differences in price and sensory characteristics between these two species, the identification of the presence of each species in commercial blends is of great interest. The aim of this study was to describe typical profiles of caffeine and diterpenes (kahweol and cafestol) contents and the ratios among these compounds to support the characterization of Coffea species in roasted coffees. 32 good cup quality Brazilian C. arabica coffees (from coffee quality contests) produced using different postharvest treatments were studied. All analysis were performed by HPLC. Higher ranges were observed in diterpene contents - kahweol varied from 1.75 to 10.68 g/kg (coefficient of variation of 510%) and cafestol from 1.76 to 9.66 g/kg (449%) - than caffeine, that varied from 5.1 to 16.2 g/kg (coefficient of variation of 218%). Wide ranges of the kahweol/cafestol ratio (0.63 to 2.77) and the caffeine/kahweol ratio (0.84 to 5.15) were also observed. Hence it was proposed the additional use of a new parameter, the ratio of caffeine/sum of diterpenes (kahweol + cafestol) that presents values from 0.54 to 2.39. The results indicated that the combined use of these parameters could be a potential tool for discriminating Coffea species in blends of roasted and ground coffee. It was proposed as potentially indicative of C. arabica: values of kahweol/cafestol ratio above 0.50, associated with caffeine/kahweol ratio lower than 5.50 and caffeine/sum of diterpenes ratio lower than 2.50.

Physico-elemental analysis of roasted organic coffee beans from Ethiopia, Colombia, Honduras, and Mexico using X-ray micro-computed tomography and external beam particle induced X-ray emission.

The physico-elemental profiles of commercially attained and roasted organic coffee beans from Ethiopia, Colombia, Honduras, and Mexico were compared using light microscopy, X-ray micro-computed tomography, and external beam particle induced X-ray emission. External beam PIXE analysis detected P, S, Cl, K, Ca, Ti, Mn, Fe, Cu, Zn, Br, Rb, and Sr in samples. Linear discriminant analysis showed that there was no strong association between elemental data and production region, whilst a heatmap combined with hierarchical clustering showed that soil-plant physico-chemical properties may influence regional elemental signatures. Physical trait data showed that Mexican coffee beans weighed significantly more than beans from other regions, whilst Honduras beans had the highest width. X-ray micro-computed tomography qualitative data showed heterogeneous microstructural features within and between beans representing different regions. In conclusion, such multi-dimensional analysis may present a promising tool in assessing the nutritional content and qualitative characteristics of food products such as coffee.

Cold Plasma Treatment as an Alternative for Ochratoxin a Detoxification and Inhibition of Mycotoxigenic Fungi in Roasted Coffee.

Ochratoxin A (OTA) produced by mycotoxigenic fungi (Aspergillus and Penicillium spp.) is an extremely toxic and carcinogenic metabolite. The use of cold plasma to inhibit toxin-producing microorganisms in coffee could be an important alternative to avoid proliferation of mycotoxigenic fungi. Roasted coffee samples were artificially inoculated with A. westerdijikiae, A. steynii, A. versicolor, and A. niger, and incubated at 27 °C over 21 days for OTA production. Samples were cold plasma treated at 30 W input power and 850 V output voltage with helium at 1.5 L/min flow. OTA production in coffee was analyzed by high performance liquid chromatography coupled to a mass spectrometer (HPLC-MS). After 6 min of treatment with cold plasma, fungi were completely inhibited (4 log reduction). Cold plasma reduces 50% of OTA content after 30 min of treatment. Toxicity was estimated for extracts of artificially contaminated roasted coffee samples using the brine shrimp (Artemia salina) lethality assay. Toxicity for untreated roasted coffee was shown to be "toxic", while toxicity for cold plasma treated coffee was reduced to "slightly toxic". These results suggested that cold plasma may be considered as an alternative method for the degradation and reduction of toxin production by mycotoxigenic fungi in the processing of foods and feedstuffs.

The typicity of coffees from different terroirs determined by groups of physico-chemical and sensory variables and multiple factor analysis.

Coffee production is the result of the relationship between local environmental conditions and coffee cultivars that grow in this place. Coffee plants develop original physico-chemical and sensory characteristics that together with the agricultural techniques practiced by growers define the terroir. The objective of this study was to describe the typicity of coffee prepared by coffee growers from seven coffee terroirs in Paraná, Brazil. The terroir categorization was based on the local latitude, longitude, altitude and annual average temperature. Coffee samples were prepared by the coffee growers according to their agricultural techniques. A multiple factor analysis (MFA) was applied to the groups of variables of the green and roasted coffee bean physico-chemical and sensory attributes. The variability in environmental conditions was sufficient to modify the green and roasted coffee bean characteristics and sensory attributes. The terroir description obtained with MFA description compared to that obtained with individual groups of variables was different among terroirs. Roasted coffee variables and sensory attributes caused the greatest differences. The individual use of these groups of variables may result in non-representative descriptions of coffee from different terroirs. Mandaguari and Ivaiporã terroirs were associated with high nitrogenous compounds content, high expansion volume and low density of roasted coffees, and the beverages showed a high turbidity and intense body. Apucarana, São Jerônimo da Serra and Ribeirão do Pinhal terroirs were associated with low lipids content, high density and low volume expansion roasted coffee, and the beverage showed intense coffee and sweet aromas and a low turbidity and body texture. In coffee from the Londrina terroir, medium nitrogenous compounds content and high sucrose and lipids contents were found. Their beverage showed a high turbidity and intense body as well as a grassy green taste and astringency. Coffee from Ribeirão Claro terroir presented high lipids and sucrose contents and low caffeine and phenolic compounds contents, and the main sensory attributes were a coffee aroma and sweet and sour tastes. In conclusion, a terroir formed by environmental conditions and agricultural techniques can produce coffee with a set of physico-chemical and sensory characteristics that define its typicity.

An 1H NMR-based metabolomic approach to compare the chemical profiling of retail samples of ground roasted and instant coffees.

The present non-targeted 1H NMR-based fingerprinting approach along with multivariate analysis established differences between representative aqueous extracts of commercial ground roasted coffee (GRC) and instant (soluble) coffee (IC) samples. The latter were prepared either by spray drying or freeze drying. When comparing a total of 33 compounds between GRC and IC, the latter product contained a remarkable increase in 5-(hydroxymethyl)furfural and carbohydrates, as well as a clear decrease in trigonelline, N-methylpyridinium, caffeine, caffeoylquinic acids and 2-furylmethanol. Furthermore, the current protocol was able to detect the subtle chemical differences between spray-dried and freeze-dried IC. The aforementioned metabolites could serve as target molecules in the attempt to preserve, as much as possible, the organoleptic and nutraceutical properties of GRC during the industrial drying processes used in the production of the two commercial types of IC.

Validation of analytical conditions for determination of polycyclic aromatic hydrocarbons in roasted coffee by gas chromatography-mass spectrometry.

Polycyclic aromatic hydrocarbons (PAHs) are of significant interest due to their genotoxicity in humans. PAHs quantification in coffee is complex since some of its compounds interfere in the chromatographic analysis, which hinders the reliable determination of the PAHs. Analytical conditions for the ultrasound extraction, purification and quantification of 16 PAHs in roasted coffee were studied. The better extraction efficiency of benzo[a]pyrene (68%) from ground-roasted coffee was achieved with a solvent ratio of Hex:MC (9:1 v/v) and three extraction periods of 20 min, followed by alkaline saponification and purification of the extracts. The detection limits were 0.85-39.32 ng mL(-1), and the quantification limits from 2.84 to 131.05 ng mL(-1), obtained for fluoranthene and chrysene, respectively. The extraction was effective for most of the analytes, with recoveries of 39.8% dibenzo[ah]anthracene and 69.0% benzo[b]fluoranthene. For coffee roasted in a spouted bed reactor, the summation of the 16 PAHs ranged from 3.5 to 16.4 µg kg(-1).

Coffee's country of origin determined by NMR: the Colombian case.

The determination of the origin of coffee beans by NMR fingerprinting has been shown promising and classification has been reported for samples of different countries and continents. Here we show that this technique can be extended and applied to discriminate coffee samples from one country against all others, including its closest neighbors. Very high classification rates are reported using a large number of spectra (>300) acquired over a two-year period. As original aspects it can be highlighted that this study was performed in fully automatic mode and with non-deuterated coffee extracts. This is achieved using a series of experiments to procure a robust suppression of the solvent peaks. As is, the method represents a cost effective opportunity for countries to protect their national productions.

On-line solid-phase extraction using a C18 minicolumn coupled to a flow injection system for determination of caffeine in green and roasted coffee beans.

A novel and fast method based on the solid phase extraction (SPE) coupled to a flow injection system for the determination of caffeine in coffee beans was developed. The caffeine extraction of coffee beans was carried out with hot water. A C18 reverse-phase mini-column was coupled to a continuous flow manifold to carry out the on-line SPE and the quantification of caffeine from aqueous extracts. Column length, retention time, elution volume, extracting solution and injection volume were evaluated. The retention time was of 90s and the elution was carried out with 400 µL of a methanol:water mixture (25:75). The proposed on-line SPE was compared against a chloroform extraction from aqueous extracts. With the proposed method the sample preparation was minimised and the sample throughput was increased (10 determination/h) because no dilution was required. Green coffee beans and beans with different roasting degree were analyzed.

Comparison of High Performance Liquid Chromatography with Fluorescence Detector and with Tandem Mass Spectrometry methods for detection and quantification of Ochratoxin A in green and roasted coffee beans

Two analytical methods for the determination and confirmation of ochratoxin A (OTA) in green and roasted coffee samples were compared. Sample extraction and clean-up were based on liquid-liquid phase extraction and immunoaffinity column. The detection of OTA was carried out with the high performance liquid chromatography (HPLC) combined either with fluorescence detection (FLD), or positive electrospray ionization (ESI+) coupled with tandem mass spectrometry (MS-MS). The results obtained with the LC-ESI-MS/MS were specific and more sensitive, with the advantages in terms of unambiguous analyte identification, when compared with the HPLC-FLD.

Determinação quantitativa das principais substâncias utilizadas para fraudar o café torrado e moído / Quantitative determination of the main substances used to defraud ground roasted coffee

E descrita uma serie de métodos, elaborados na Seção do Café do Instituto Adolfo Lutz, São Paulo, SP, para identificação e determinação quantitativa das principais substancias (açúcar, caramelo, cevada, milho, cascas de cacau e de soja) utilizadas para fraudar o café torrado e moído. São métodos simples e rápidos, posto que ao Serviço de Fiscalização local interessa a resposta de analise no mais curto espaço de tempo possível. E descrito, ainda o aspecto das substancias da fraude, num exame a lupa (aum. 20 x) (AU).

Teores de cobre em café torrado e moído e em café bebida / Copper contents in roasted and ground coffee and in brewed coffee

Cem amostras de café torrado e moído (pó), de diferentes partes do Brasil, foram analisadas para determinação de cobre pelo método de espectrofotometria de absorção atômica. Foram analisados também os cafés bebida correspondentes. Os resultados encontrados mostraram um valor médio de 17,26 p.p.m. de cobre para os pós e de 1,19 p.p.m. para os cafés bebida. Como o café bebida foi preparado de modo a representar uma diluição de 1:5 do pó correspondente, os valores encontrados indicam uma extração de 34,9% do cobre existente nos pós. 5% das amostras de pós mostraram um nivel abaixo de 10p.p.m. de cobre. Neste pós, quase todo o cobre foi extraído quando o café bebida foi obtido. Não há correlação entre os valores de cobre obtidos no café bebida e o contidos no pó. Quando os cafés bebidas foram preparados do mesmo modo (na diluição de 1:5), todos mostraram um nivel de cobre de 1,0 p.p.m.+-0,26...

Determinação do sedimento, cascas e paus no café e moido / Determination of sediment, husks and sticks in coffee and ground

Neste trabalho foi descrito método para determinação do sedimento e cascas no café de consumo, torrado e moído. Consiste no desengorduramento parcial do material com solvente para separar o sedimento e deixar o pó solto, peneração para livrar a amostra do pó (que não é de interesse na observação para livrar a amostra do pó (que não é de interesse na observação á lupa), separação das impurezas e pesagem. No calculo final, usou-se o fator de conversão para reverter o peso encontrado em peso de impurezas no café verde (AU).