Journal of the Science of Food and Agriculture

J Sci Food Agric 83:240248 (online: 2003) DOI: 10.1002/jsfa.1304

Inuence of extraction temperature on the nal quality of espresso coffee

n a Pascual, Carmen Iba Susana Andueza, Laura Maeztu, Luc ez, M Paz de Pen a n Cid* and Concepcio
a, Tecnolog a de Alimentos y Toxicolog a, Facultad de Farmacia, Universidad de Navarra, E-31080 Departamento de Bromatolog Pamplona, Spain

Abstract: The nal quality of espresso coffee (EC) depends upon certain technical conditions, such as the extraction temperature used in preparing it. The aim of this work was to investigate the effects of water temperature (88, 92, 96 and 98 C) on the nal quality of three types of EC (Arabica, Robusta Natural blend and Robusta Torrefacto blend) in order to select the optimal temperature. Volatile compound (analysed by Static headspace gas chromatography/mass spectrometry) and sensory avour proles were the most relevant parameters, whereas physicochemical, taste and mouthfeel parameters were not very useful for selecting the water temperature. For Arabica and Robusta Natural blend ECs, 92 C was the optimal water temperature. For Robusta Torrefacto blend EC the overall acceptability might lead to the selection of 88 C as the ideal water temperature, but the high percentages of key odorants related to roasty and earthy/musty avours and the not hot enough perception dictated the selection of 92 C in this case as well. # 2003 Society of Chemical Industry

Keywords: espresso coffee; coffee aroma; extraction temperature; sensory avour prole; Arabica coffee; Robusta coffee; Torrefacto roast

INTRODUCTION

Espresso coffee (EC) is a beverage prepared on request from roasted and ground coffee beans. In the espresso technique, pressure induces percolation of a limited amount of hot water through a ground coffee cake in a short time to yield a small cup of a concentrated foamy elixir.1 The preparation of EC is inuenced by factors related to the coffee and water and other technical conditions related to the machine. The effects of the variety of coffee (Arabica and Robusta) and the degree of roast on the quality of EC have been studied by several authors.25 In addition, the inuence of Torrefacto roast (roasting process with the addition of sugar) has been studied by Maeztu et al. 4 The composition of the water is another quality factor of EC preparation which has been studied by Illy and Viani2 and Navarini et al. 6 Obviously, the physical, chemical and sensory (or organoleptic) properties of EC depend upon certain technical conditions in its preparation. Some of them, such as size of coffee particles, water/coffee ratio, water temperature and contact time between coffee and water, have been reported for coffee brews.2,79 However, the effects of

other specic technical conditions on the quality of EC, such as water pressure and temperature, extraction time and holder lter diameter, have been less well studied.2,10 Water temperature is one of the greatest inuences on the nal quality of EC, because hot water can extract many different chemical compounds from the roasted and ground coffee. Some substances are volatile and are responsible for the aroma (aldehydes, ketones, pyrazines, etc). Others are soluble and nonvolatile and can be considered as the taste source (caffeine, trigonelline, acids, sugars, etc). The extracted insoluble compounds become the coffees body and foam (proteins, polysaccharides and melanoidines). An adequate extraction produces a good espresso which should have a balanced bitter/acid taste, a strong body, a full ne aroma, a pleasant aftertaste and a large amount of persistent, consistent and hazelnut foam with a tiger-skin effect.2,11 A temperature that is not hot enough could decrease the coffee extraction, producing a weaker and less aromatic EC. A wide water temperature range of 8595 C has been suggested by Petracco1 and Illy and Viani.2

n Cid, Departamento de Bromatolog a, Tecnolog a de Alimentos y Toxicolog a, Facultad de Farmacia, * Correspondence to: Concepcio Universidad de Navarra, E-31080 Pamplona, Spain E-mail: ccid@unav.es Part of this paper was presented at the 19th International Conference on Coffee Science, Trieste, Italy n Interministerial de Ciencia y Tecnolog a; contract/grant number: ALI-1999-0319 Contract/grant sponsor: Comisio Contract/grant sponsor: Departamento de Industria del Gobierno de Navarra a Espan Contract/grant sponsor: Ministerio de Ciencia y Tecnolog ol (Received 19 June 2002; revised version received 27 August 2002; accepted 14 October 2002)

# 2003 Society of Chemical Industry. J Sci Food Agric 00225142/2003/$30.00

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Extraction temperature of espresso coffee

Control of the water temperature is essential in order to obtain a high-quality espresso coffee, because it plays an integral role in the extraction of taste, body and volatile avour compounds, but this is very difcult in a commercial espresso machine. Therefore the development of an experimental EC prototype machine which would allow the control of all cited technical conditions was necessary for this study. The aim of this work was to investigate the effects of water temperature on the nal quality of three types of EC in order to choose the optimal temperature. Moreover, this study provided us with EC parameters and attributes which might be relevant to the quality of a good EC.

Total solids, extraction and total solids in ltrate

Total solids were determined by oven drying 40 ml of EC (with foam) to a constant weight (14 h, 102 (3) C). Extraction was dened as the percentage of total solids with respect to the ground roasted coffee dose (7.5 g). Total solids in ltrate were determined by oven drying 40 ml of EC, after ltering with Whatman No 1 paper, to a constant weight (14 h, 102 (3) C).
Lipids

EXPERIMENTAL Materials

Total lipids were determined by liquidliquid extraction with trichloromethane. A 20 ml volume of EC (with foam) was extracted by adding 20 ml of trichloromethane three times in a separating funnel. The organic fraction was washed with distilled water three times. Total lipids were quantied by weight after evaporation of the solvent.
Caffeine and trigonelline

Three roasted coffee samples, Arabica (pure Coffea arabica from Colombia, 2.0% water content), Robusta Natural blend (80:20 blend of C canephora and C arabica, 2.0% water content) and Robusta Torrefacto blend (50% Robusta Natural blend, previously dened, and 50% Robusta Torrefacto roast, 1.8% water content), were provided by a local factory. Two batches of each coffee sample were used. Pure reference standards of acetaldehyde, 2-methylpropanal, 3-methylbutanal, 2,3-butanedione, 2,3pentanedione and 2-ethyl-3,5-dimethylpyrazine were purchased from Acros (NJ, USA); hexanal, guaiacol and propanal were obtained from Sigma (Steinheim, Germany).
EC samples and preparation for analysis

Extract preparation and clean-up and high-performance liquid chromatography (HPLC) analysis have already been described by Maeztu et al. 4 HPLC analysis was achieved with an analytical HPLC unit (Hewlett Packard (HP) 1100) equipped with a Rheodyne injector of 20 ml loop, a binary pump and a diode array detector. A reverse phase Hypersil-ODS column (5 mm particle size, 250 mm 4.6 mm) was used. The mobile phase was acetonitrile/water (15:85) in isocratic condition at a constant ow rate of 2.0 ml min1 at 25 C. Detection was accomplished with a diode array detector, and chromatograms were recorded at 280 nm.
Chlorogenic acid (5-CQA)

The ECs were prepared from 7.5 g of nely ground roasted coffee for a volume of 40 ml, with the use of an experimental EC prototype machine. EC preparation conditions were xed at 9 atm relative water pressure, 21 3 s extraction time and 38 mm holder lter diameter. Water temperatures (before crossing the ground coffee) studied were 88, 92, 96 and 98 C, corresponding to erogation (coffee extraction) temperatures of 82 2, 86 2, 90 2 and 92 (2) C respectively. Twenty ECs of each coffee sample were prepared for physicochemical analysis in triplicate.
pH, density, viscosity and surface tension

The extraction of 5-CQA and clean-up were carried out according to Bicchi et al. 12 The HPLC equipment has been described previously. The conditions of the gradient solvent system used were 100% citrate/acetic acid buffer solution (pH 3.0) for 2 min, 85:15 buffer/ methanol for 8 min, both at a ow rate of 0.8 ml min1, and 85:15 buffer/methanol for 5 min at a ow rate of 1.2 ml min1, at 25 C. The wavelength of detection was 325 nm.
Sensory descriptive analysis

The EC samples were rapidly cooled at 20 C and the pH (Orion 420A benchtop pH meter), density (densimeter), viscosity (Ostwald viscosimeter) and surface tension (Traube estalagmometer) were measured.
Foam index and persistence of foam

The foam index was dened as the ratio (%) of EC foam and liquid volumes measured immediately after the extraction of EC using a 100 ml graduated cylinder. The persistence of foam was dened as the time (min) that the liquid phase below the cream layer took to appear during cooling at room temperature.
J Sci Food Agric 83:240248 (online: 2003)

The sensory properties of the EC samples were measured using a variation of the quantitative descriptive analysis (QDA) method.13 Twenty judges were recruited from members of the Food Science and Technology Department at the University of Navarra. Selection and training were carried out using the method described by Maeztu et al. 4 The appearance of foam was dened by colour (clear, hazelnut or dark), consistency (consistent or inconsistent) and persistence (with a hole in the centre, evanescent or persistent) as the percentage of judges that observed each attribute. For attributes such as odour intensity, body, acidity, bitterness, astringency, avour intensity and aftertaste intensity, 10 cm linear scales, typically anchored with the words
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none (0) and very high (10) about 1 cm from each end and marked in the middle with medium (5), were used. Means and standard deviations for each attribute in each EC sample were obtained. A sensory avour prole was included on the same scorecard. The most frequent odour/avour attributes described by judges during the training process were written in two columns, one for positive and the other for negative avour attributes. Positive avour attributes were fruity/winey, malty/cereal, freshness, straw, caramel-like, chocolate-like, spicy, nutty, tobacco and buttery. Negative avour attributes were woody/ papery, burnt/roasty, acrid, fermented, earthy/musty, rancid, burnt rubbery, sulphurous, at, grassy/green/ herbal, animal-like, motor-oily and ashy. In both columns, one line for other avours was added. The avour prole of each EC sample was dened by the percentage of judges that perceived each positive and negative avour attribute. Descriptive evaluation of the EC samples was then carried out in triplicate over 24 sessions. Three ECs were analysed per session. Each EC was prepared immediately before tasting, and served in a white porcelain coffee cup labelled with a three-digit code. The order of presentation was randomised among judges and sessions. All evaluations were conducted in isolated sensory booths illuminated with white light in the sensory lab under standardised conditions (UNE 87-004-79).14 Rinse water was provided between individual samples.
Overall acceptability

The injector temperature was set at 180 C, and helium (10 ml min1 linear speed) was the carrier gas. The oven temperature was maintained at 40 C for 6 min and then programmed to 190 C at 3 C min1. Mass spectrometry analysis was carried out using an HP 5973 mass-selective detector coupled to the gas chromatograph. The mass spectrometer was operated in electron impact ionisation mode (70 eV) with a scan range of 33300 amu. The ion source temperature was set at 230 C. Identification of volatile compounds The volatile compounds studied were identied by comparing their mass spectra with those in the Wiley library and, in addition, by comparison of their retention times with those of standard compounds. The Kovats indices were also calculated according to Tranchant16 and compared with available literature data.17 Quantitative measurements Methanethiol, acetaldehyde, propanal, 2-methylpropanal, 2-methylbutanal, 3-methylbutanal, 2,3-butanedione, 2,3-pentanedione, hexanal, 2-ethylpyrazine, 2-ethyl-6-methylpyrazine, 2-ethyl-3,5-dimethylpyrazine and guaiacol were quantied as key odorants. The content of key odorants of each headspace analysis was quantied by integrating the peak areas of the 13 compounds studied. Areas of peaks were measured by calculation of the total area based on integration of a single ion. The relative percentages of individual compounds were calculated from the total contents of volatiles on the chromatograms.
Statistical analysis

The overall acceptability was evaluated by consumers using a 10 cm linear structured scale anchored with the words very bad (0) and very good (10) about 1 cm from each end. Overall acceptability testing of the EC samples was carried out in triplicate. Each EC was prepared immediately before tasting, and served in a white porcelain coffee cup labelled with a three-digit code. The order of presentation was randomised among consumers. Means for each EC sample were obtained.
Volatile compounds

Analysis of variance (ANOVA) was applied to the physicochemical and sensory data and volatile compounds. The source of variation was the temperature of the water. Tukeys t-test was applied a posteriori with a level of signicance of 95%. All statistical analyses were performed using the SPSS v 10.0 software package.

The proles of volatile compounds were obtained with the method described by Sanz et al,15 adapted to EC and using static headspace gas chromatography/mass spectrometry (SH-GC/MS). SH-GC analysis was performed with an HP 6890 gas chromatograph equipped with an HP 7694 static headspace sampler. A 6 ml volume from a homogenised EC cup was introduced into a 10 ml vial, which was immediately sealed with a silicone rubber Teon cap. Each vial was equilibrated at 60 C (the temperature at which EC is drunk) for 20 min in the static headspace sampler. Each vial was pressurised with carrier gas for 12 s, and 3 ml of the coffee headspace sample was injected into an HP-Wax capillary column (60 m 0.25 mm, 0.5 mm lm thickness). Each EC sample was analysed in triplicate, using three EC cups.
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RESULTS AND DISCUSSION

Physicochemical, sensory and overall acceptability results for all EC samples are summarised in Tables 1 and 2 and Fig 5, while Tables 35 and Figs 24 show the results of key odorants and avour notes for each type of EC separately.
Inuence of water temperature on physicochemical parameters and sensory attributes of EC samples

Signicant increases in total solids and total solids in ltrate, and therefore extraction were found when the temperature was increased (Table 1). Lingle18 proposed that extraction percentages should be in the range 1822% (180220 g kg1) in order to obtain a coffee beverage with the most desirable avours. When extraction is above 22% (220 g kg1), the coffee
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Extraction temperature of espresso coffee

pH 5.3; 0.0a 5.4; 0.1b 5.4; 0.0b 5.4; 0.0b 5.7; 0.0ab 5.7; 0.0b 5.6; 0.1a 5.6; 0.0ab 5.6; 0.0b 5.6; 0.0b 5.6; 0.0b 5.4; 0.1a 1.010; 0.000a 1.010; 0.000a 1.010; 0.000a 1.010; 0.000a 1.010; 0.000a 1.010; 0.000a 1.010; 0.000a 1.010; 0.000a 1.010; 0.000b 1.010; 0.000b 1.010; 0.000a 1.010; 0.000b Density (g ml 1) 1.26; 0.06a 1.25; 0.03a 1.35; 0.11a 1.29; 0.03a 1.21; 0.08a 1.24; 0.07a 1.26; 0.04a 1.24; 0.10a 1.16; 0.05a 1.21; 0.03a 1.29; 0.07b 1.23; 0.07ab Viscosity (mN m2 s1) 49.4; 2.1a 49.6; 1.3a 50.0; 1.0a 50.1; 2.0a 51.0; 0.0a 50.5; 0.2a 50.3; 1.6a 45.5; 1.3a 46.2; 2.0a 45.8; 2.3a 51.6; 1.8b Surface tension (mN m1) 49.3; 0.8a Foam index (%) 12.1; 0.2a 12.3; 0.1a 12.3; 0.2a 12.8; 0.2b 17.4; 0.3a 17.5; 0.3a 20.3; 0.5b 21.0; 0.7c 18.4; 0.0a 20.4; 0.4b 22.3; 0.6c 23.9; 0.8d Persistence of foam (min) 26.2; 1.0a 28.2; 2.2a 30.0; 4.6a 27.2; 3.1a 24.0; 0.6a 23.7; 2.3a 24.5; 2.8a 25.8; 1.3a 30.0; 0.0a 28.5; 2.4a 28.4; 1.2a 27.5; 2.7a 35.9; 0.5a 39.2; 0.8b 41.7; 1.0c 41.6; 0.3c 37.7; 0.2a 38.1; 0.1a 39.7; 1.4b 40.3; 1.5b 42.4; 0.6a 43.3; 0.6b 43.6; 0.8b 43.7; 0.1b Total solids (mg ml 1) 192; 0.3a 209; 0.5b 222; 0.5c 222; 0.2c 199; 0.2a 203; 0.1a 212; 0.7b 215; 0.8b 226; 0.3a 231; 0.3b 233; 0.4b 233; 0.0b Extraction (g kg1) 34.7; 0.3a 37.4; 0.7b 39.1; 1.3c 40.3; 0.2c 36.7; 0.4a 36.8; 0.6a 38.5; 1.5b 38.7; 1.3b 40.9; 0.4a 41.1; 0.4a 42.0; 0.8b 41.9; 0.1b Total solids in ltrate (mg ml 1) Total lipids (mg ml 1) 4.93; 0.03a 5.15; 0.03b 5.86; 0.24c 6.06; 0.02d 4.45; 0.16b 3.97; 0.27a 4.77; 0.42bc 4.96; 0.16c 4.16; 0.03a 4.32; 0.09b 4.35; 0.19b 4.73; 0.03c 2.02; 0.03a 2.05; 0.03a 2.09; 0.10a 2.31; 0.13b 3.03; 0.05a 3.05; 0.13a 2.94; 0.08a 3.02; 0.10a 2.90; 0.05a 2.89; 0.08a 2.96; 0.06a 2.92; 0.04a Caffeine (mg ml 1) 0.81; 0.10a 0.94; 0.02b 1.15; 0.07c 1.39; 0.02d 1.16; 0.22a 1.30; 0.14b 1.08; 0.02a 1.07; 0.16a 0.97; 0.05b 1.34; 0.10c 1.33; 0.11c 0.79; 0.09a Trigonelline (mg ml 1) 1.12; 0.02c 1.01; 0.04b 0.92; 0.02a 1.47; 0.03b 1.27; 0.10a 1.32; 0.05a 1.35; 0.06a 0.97; 0.02a 1.11; 0.05c 1.05; 0.02b 1.08; 0.03bc Chlorogenic acid (5-CQA) 1.01; 0.02b (mg ml 1)

Robusta Natural blend

All values are shown as mean; standard deviation of mean (n = 6). In each row, different superscripts indicate signicant differences (p < 0.05) among different temperatures of extraction for each coffee type.

beverage tends to have an unpleasant, astringent and very bitter taste and could be considered overextracted. In our study the percentages of extraction for 96 and 98 C Arabica and all Robusta Torrefacto blend EC samples were outside this range. Also, these samples were perceived as more astringent and bitter by the panel of judges (Table 2). In Robusta Torrefacto blend EC samples the higher percentage of extraction could be produced by extracted caramelised sugar which had been added during the roasting process. Therefore the percentage of extraction should be revised when Torrefacto roasted coffee is used, allowing a value higher than 22% (220 g kg1) to be considered acceptable. Among the physical parameters, only the foam index increased. This might be due to the high extraction of total solids. In all samples the foam index was higher than 10%, the minimum value proposed by Illy and Viani2 for a good EC. Other extracted compounds, such as total lipids and caffeine, tended to increase with water temperature. However, in general, the extraction of trigonelline and chlorogenic acid increased until 92 C was reached and then tended to decrease with further increase in temperature, because they could break up into other compounds.
Inuence of water temperature on aroma/avour of EC samples

Robusta Torrefacto blend

92 C

96 C

98 C

88 C

92 C

96 C

98 C

A typical gas chromatogram obtained for the three types of EC sample prepared at 92 C is shown in Fig 1. Thirteen key odorants were quantied according to the results obtained by several authors who applied aroma extract dilution analysis (AEDA), gas chromatography/olfactometry of headspace (GC/OH)1922 and correlations between SH-GC/MS and sensory analysis.5 Consequently, for each type of EC, one table for key odorants and one gure for avour notes are shown. Methanethiol has been related to freshness aroma in ground roasted coffee23 and to sulphurous avour in coffee brew.20 Acetaldehyde and propanal may be responsible for fruity avour in coffee brew.5,20 2-Methylpropanal, 2-methylbutanal and 3-methylbutanal, Strecker degradation products of valine, isoleucine and leucine, were suggested to be the compounds responsible for malty avour in coffee brew.20,24 2,3-Butanedione and 2,3-pentanedione were associated with buttery avour.19,20 On the other hand, hexanal is responsible for green aroma.22 Pyrazines have been associated with roasty and earthy/musty avours in ground roasted coffee and coffee brew.5,19,22 Guaiacol, a phenolic compound, is responsible for phenolic,19,22 spicy19 and burnt20 aromas/avours. Arabica EC aroma/avour results are shown in Table 3 and Fig 2. The highest values for sulphur compounds, aldehydes and ketones and the lowest ones for pyrazines were obtained at 92 C. All odorants related to freshness, fruity, malty and buttery
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Table 1. Inuence of water temperature on physicochemical parameters of espresso coffee samples

Arabica Parameter 88 C 92 C

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96 C

98 C

88 C

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Table 2. Inuence of water temperature on sensory attributes of espresso coffee samples

Arabica Attribute Odour intensity Body Acidity Bitterness Astringency Flavour intensity Aftertaste intensity 88 C 92 C 96 C 6.1; 1.0b 5.6; 6.0; 6.6; 6.2; 6.4; 0.7b 1.4b 0.7ab 0.8ab 1.2b 98 C 88 C

Robusta Natural blend 92 C 96 C 98 C 88 C

Robusta Torrefacto blend 92 C 96 C 6.2; 1.0b 6.3; 0.8; 7.4; 6.9; 6.6; 1.4b 0.3a 1.2ab 1.2ab 1.2b 98 C 6.4; 1.2b 6.1; 1.8; 7.7; 7.3; 6.7; 1.0b 0.4b 1.0b 1.3b 1.0b

5.7; 0.9a 6.3; 0.8b 4.7; 5.1; 6.1; 5.7; 6.0; 0.6a 1.4a 1.5a 1.4a 0.8a 5.5; 6.0; 6.3; 6.0; 6.7; 0.8b 1.2b 1.2ab 1.4ab 0.8b

6.7; 0.9c 5.6; 0.9a 5.7; 0.8a 5.8; 1.0a 6.0; 1.2a 5.5; 1.0a 6.1; 1.1b 6.0; 5.9; 6.8; 6.3; 6.7; 0.9c 1.7b 1.4b 0.7b 1.0b 5.5; 1.4; 6.9; 6.3; 6.1; 1.1a 0.6a 1.1a 1.0a 0.9a 5.6; 1.3; 7.5; 6.4; 6.1; 0.9a 0.6a 1.1b 1.3a 1.0a 5.5; 1.9; 7.3; 6.6; 6.1; 1.0a 0.4b 1.5b 1.1a 1.1a 6.3; 1.9; 7.8; 6.6; 6.3; 1.0b 0.4b 0.9b 1.2a 1.2a 5.5; 2.9; 7.1; 6.7; 6.1; 1.1a 0.6c 0.7a 1.1a; 1.1a 6.2; 1.9; 7.2; 7.1; 6.8; 0.8b 0.7b 1.3a 1.0ab 0.9b

5.8; 0.9b 5.8; 0.9b

5.3; 1.3a

6.0; 0.9b 6.6; 1.0a 6.6; 1.2a 6.2; 1.0a 6.7; 1.0a 6.5; 1.1a 6.7; 1.2a

6.9; 1.2a

6.7; 1.3a

All values are shown as mean; standard deviation of mean (n = 6). In each row, different superscripts indicate signicant differences (p < 0.05) among different temperatures of extraction for each coffee type.

Figure 1. Typical gas chromatogram of espresso coffee sample prepared at 92 C: 1, methanethiol; 2, acetaldehyde; 3, propanal; 4, 2-methylpropanal; 5, 2-methylbutanal; 6, 3-methylbutanal; 7, 2,3-butanedione; 8, 2,3-pentanedione; 9, hexanal; 10, 2-ethylpyrazine; 11, 2-ethyl-6-methylpyrazine; 12, 2-ethyl-3,5-dimethylpyrazine; 13, guaiacol.

avours, except 2-methylbutanal and 2,3-butanedione, were signicantly lower in 88 than in 92 C Arabica EC. The 88 C samples were perceived by the panel of judges as having lower odour, avour and body intensities in comparison with higher-tempera-

ture samples. Also, these EC samples had lower overall acceptability values (see Fig 5). No signicant differences in sulphur compounds, aldehydes and ketones between 92 and 96 C Arabica ECs were found, with the exception of acetaldehyde and 3-

Table 3. Inuence of water temperature on key odorants of Arabica espresso coffee samples (% compound area/total area)

KI 635 645 712 747 880 884 962 1058 1084 1359 1411 1475

ID C A A A C A A A A C C A A

Key odorant Methanethiol Acetaldehyde Propanal 2-Methylpropanal 2-Methylbutanal 3-Methylbutanal 2,3-Butanedione 2,3-Pentanedione Hexanal 2-Ethylpyrazine 2-Ethyl-6-methylpyrazine 2-Ethyl-3,5-dimethylpyrazine Guaiacol

88 C 0.05; 0.00a 0.34; 0.02a 0.47; 0.03a 1.84; 0.09a 1.41; 0.04a 2.62; 0.27a 0.45; 0.05a 0.59; 0.05a 0.08; 0.02b 0.07; 0.01a 0.04; 0.01a 0.01; 0.00a 0.1; 0.16a

92 C 0.11; 0.41; 0.57; 2.31; 1.53; 3.54; 0.50; 0.74; 0.07; 0.07; 0.04; 0.01; 0.02; 0.01c 0.05b 0.06b 0.38b 0.20ab 0.45c 0.08a 0.14b 0.01b 0.01a 0.01a 0.00a 0.01a

96 C 0.13; 0.34; 0.52; 2.19; 1.58; 3.11; 0.42; 0.63; 0.05; 0.10; 0.06; 0.03; 0.01; 0.01d 0.00a 0.07ab 0.05b 0.05b 0.12b 0.04a 0.04ab 0.01a 0.02b 0.01b 0.01b 0.00a

98 C 0.10; 0.38; 0.54; 2.26; 1.60; 3.15; 0.48; 0.67; 0.07; 0.07; 0.04; 0.01; 0.01; 0.01b 0.01a 0.02ab 0.08b 0.08b 0.14bc 0.02a 0.05ab 0.01b 0.01a 0.00a 0.00a 0.00a

All values are shown as mean; standard deviation of mean (n = 6). In each row, different superscripts indicate signicant differences (p < 0.05) among different temperatures of extraction. KI, Kovats index calculated for the HP-Wax capillary column. The reliability of the identication (ID) proposal is indicated by the following: A, mass spectrum, retention time and Kovats index according to standards; B, mass spectrum and Kovats index according to literature data; C, mass spectrum compared with Wiley mass spectral database.

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Figure 2. Inuence of water temperature on avour characteristics of Arabica espresso coffee samples. For each characteristic, different letters indicate signicant differences (p < 0.05) among different temperatures of extraction.

Figure 3. Inuence of water temperature on avour characteristics of Robusta Natural blend espresso coffee samples. For each characteristic, different letters indicate signicant differences (p < 0.05) among different temperatures of extraction.

methylbutanal. In contrast, the contents of pyrazines were signicantly increased with a water temperature of 96 C and these could be the origin of the highest burnt/roasty avour perceived by the judges. Although only hexanal increased in 98 C Arabica EC, a higher percentage of judges perceived negative avour notes, such as woody/papery, burnt/roasty and acrid, which might be produced by other unidentied negative key odorants. The best prole of key odorants and avour notes, a persistent, consistent and hazelnut foam with a tigerskin effect and the highest overall acceptability (see Fig 5) were obtained for 92 C Arabica EC. Therefore

92 C was considered to be the optimal temperature for the preparation of a good Arabica EC. Robusta Natural blend EC aroma/avour results are shown in Table 4 and Fig 3. The sensory characteristics of Robusta Natural blend EC samples were very similar at all temperatures. The highest percentages of key odorants related to freshness, fruity, malty and buttery avours in Robusta Natural blend EC were obtained at 92 C, while the highest percentages of key odorants related to roasty and earthy/musty avours were extracted at 96 C. Robusta Natural blend ECs made at 88 and 92 C were similar in physicochemical and sensory characteristics, key odorants related to

Table 4. Inuence of water temperature on key odorants of Robusta Natural blend espresso coffee samples (% compound area/ total area)

KI 635 645 712 747 880 884 962 1058 1084 1359 1411 1475

ID C A A A C A A A A C C A A

Key odorant Methanethiol Acetaldehyde Propanal 2-Methylpropanal 2-Methylbutanal 3-Methylbutanal 2,3-Butanedione 2,3-Pentanedione Hexanal 2-Ethylpyrazine 2-Ethyl-6-methylpyrazine 2-Ethyl-3,5-dimethylpyrazine Guaiacol

88 C 0.11; 0.33; 0.44; 2.65; 2.07; 2.50; 0.33; 0.42; 0.04; 0.13; 0.10; 0.05; 0.03; 0.01b 0.02a 0.02ab 0.41a 0.42b 0.31a 0.02a 0.05ab 0.01ab 0.04a 0.02a 0.05ab 0.00c

92 C 0.11; 0.35; 0.51; 2.76; 2.01; 2.96; 0.33; 0.42; 0.05; 0.11; 0.08; 0.04; 0.02; 0.01b 0.07a 0.10b 0.51a 0.36ab 0.60a 0.02a 0.03b 0.01b 0.02a 0.00a 0.03ab 0.00b

96 C 0.01; 0.30; 0.39; 2.37; 1.86; 2.50; 0.31; 0.37; 0.03; 0.17; 0.12; 0.07; 0.01; 0.00a 0.01a 0.01a 0.02a 0.00ab 0.15a 0.00a 0.01ab 0.01a 0.01b 0.02b 0.00b 0.00ab

98 C 0.10; 0.31; 0.38; 2.37; 1.55; 2.57; 0.33; 0.36; 0.04; 0.12; 0.08; 0.01; 0.01; 0.03b 0.06a 0.04a 0.40a 0.30a 0.54a 0.07a 0.05a 0.01ab 0.02a 0.02a 0.00a 0.00a

All values are shown as mean; standard deviation of mean (n = 6). In each row, different superscripts indicate signicant differences (p < 0.05) among different temperatures of extraction. KI, Kovats index calculated for the HP-Wax capillary column. The reliability of the identication (ID) proposal is indicated by the following: A, mass spectrum, retention time and Kovats index according to standards; B, mass spectrum and Kovats index according to literature data; C, mass spectrum compared with Wiley mass spectral database.

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Table 5. Inuence of water temperature on key odorants of Robusta Torrefacto blend espresso coffee samples (% compound area/total area)

KI 635 645 712 747 880 884 962 1058 1084 1359 1411 1475

ID C A A A C A A A A C C A A

Key odorant Methanethiol Acetaldehyde Propanal 2-Methylpropanal 2-Methylbutanal 3-Methylbutanal 2,3-Butanedione 2,3-Pentanedione Hexanal 2-Ethylpyrazine 2-Ethyl-6-methylpyrazine 2-Ethyl-3,5-dimethylpyrazine Guaiacol

88 C 0.05; 0.20; 0.31; 1.71; 1.39; 1.81; 0.23; 0.30; 0.03; 0.15; 0.10; 0.02; 0.03; 0.01a 0.02a 0.01a 0.07a 0.06a 0.13a 0.02a 0.02a 0.01a 0.04c 0.03c 0.00b 0.00b

92 C 0.10; 0.24; 0.34; 1.80; 1.32; 2.02; 0.26; 0.34; 0.03; 0.10; 0.06; 0.01; 0.02; 0.01b 0.02b 0.02b 0.17a 0.13a 0.15b 0.02a 0.03a 0.01a 0.01ab 0.00ab 0.00a 0.00a

96 C 0.06; 0.23; 0.32; 1.61; 1.25; 2.08; 0.25; 0.31; 0.03; 0.13; 0.08; 0.06; 0.07; 0.01a 0.01b 0.02ab 0.05a 0.04a 0.06b 0.02a 0.03a 0.00a 0.02bc 0.01bc 0.01b 0.00c

98 C 0.10; 0.22; 0.31; 1.78; 1.41; 2.11; 0.24; 0.31; 0.03; 0.08; 0.05; 0.01; 0.01; 0.02b 0.02ab 0.02ab 0.13a 0.16a 0.19b 0.03a 0.05a 0.01a 0.01a 0.01a 0.00a 0.00a

All values are shown as mean; standard deviation of mean (n = 6). In each row, different superscripts indicate signicant differences (p < 0.05) among different temperatures of extraction. KI, Kovats index calculated for the HP-Wax capillary column. The reliability of the identication (ID) proposal is indicated by the following: A, mass spectrum, retention time and Kovats index according to standards; B, mass spectrum and Kovats index according to literature data; C, mass spectrum compared with Wiley mass spectral database.

positive avours, and avour notes. Only the three pyrazines decreased at 92 C. Nevertheless, the panel of judges perceived that 88 C Robusta Natural blend EC was not hot enough, and the consumers gave it a lower overall acceptability rating (see Fig 5). Of the two water temperatures, 92 C appeared to be the better one. When the water temperature rose to 96 C, the percentage of judges that perceived negative avour notes, mainly burnt/roasty and acrid, was signicantly higher. When the temperature increased further to 98 C, burnt rubbery avour was also perceived. Moreover, in 96 and 98 C Robusta Natural blend ECs the judges perceived that the foam was darker. In comparison with Arabica EC, fewer positive avour notes and higher percentages of negative avour were perceived owing to the addition of Robusta coffee. The best prole of key odorants and avour notes, a persistent, consistent and hazelnut foam and the

highest overall acceptability (see Fig 5) were obtained for 92 C Robusta Natural blend EC. Therefore the optimal water temperature for obtaining a good Robusta Natural blend EC was 92 C. Robusta Torrefacto blend EC aroma/avour results are shown in Table 5 and Fig 4. The prole of odorants related to freshness, fruity, malty and buttery avours was similar among the different water temperatures. However, the highest values for key odorants related to roasty and earthy/musty avours were obtained at 88 and 96 C. In every Robusta Torrefacto blend EC the panel of judges perceived a great variety of negative avour notes, which signicantly increased at 96 and 98 C. The increase in the number of negative avour notes in Robusta Torrefacto blend EC could be due to an increase in other key odorants not identied under our HS-GC/MS conditions. A Torrefacto roasting process is usually applied to increase the body and mask the low quality of some

Figure 4. Inuence of water temperature on avour characteristics of Robusta Torrefacto blend espresso coffee samples. For each characteristic, different letters indicate signicant differences (p < 0.05) among different temperatures of extraction.

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Extraction temperature of espresso coffee

Figure 5. Inuence of water temperature on overall acceptability of espresso coffee samples. For each coffee type, different letters indicate signicant differences (p < 0.05) among different temperatures of extraction.

Robusta coffees, but in our work the avour sensory prole observed in Robusta Torrefacto blend EC was worse than that found in Robusta Natural blend EC. The lowest percentage of negative avour notes and the highest overall acceptability (Fig 5) might lead to the selection of 88 C as the ideal water temperature. However, the low body, avour and odour intensities, the high percentages of key odorants related to roasty and earthy/musty avours and the not hot enough perception dictated the selection of 92 C as the optimal temperature for making the most acceptable Robusta Torrefacto blend EC.

CONCLUSIONS

The best qualities of our three samples of EC (Arabica, Robusta Natural blend and Robusta Torrefacto blend) were found when the water temperature was 92 C. The best prole of key odorants and avour notes and the highest overall acceptability were obtained at this temperature. For the selection of the optimal water temperature, the volatile compound (analysed by HS-GC/MS) and sensory avour proles were the most relevant parameters.

ACKNOWLEDGEMENTS

n Interministerial de Ciencia y We thank the Comisio a (project ALI-1999-0319) for its contribuTecnolog tion to the nancial support of this work. We also thank the Departamento de Industria del Gobierno de a Navarra and the Ministerio de Ciencia y Tecnolog ol for the grants given to L Maeztu and S Espan Andueza respectively. Finally, we thank the panel of judges, without whom this study could not have been carried out.

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