Jackfruit volatile compounds were established using solid-phase microextraction (SPME) and gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) thirty-seven compounds were identified from five jackfruit cultivars.
Jackfruit volatile compounds were established using solid-phase microextraction (SPME) and gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) thirty-seven compounds were identified from five jackfruit cultivars.
Jackfruit volatile compounds were established using solid-phase microextraction (SPME) and gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) thirty-seven compounds were identified from five jackfruit cultivars.
Analysis of volatile compounds in ve jackfruit (Artocarpus heterophyllus L.)
cultivars using solid-phase microextraction (SPME) and gas chromatography-time-of-ight mass spectrometry (GC-TOFMS) B.T. Ong a , S.A.H. Nazimah a, , C.P. Tan b , H. Mirhosseini b , A. Osman a , D. Mat Hashim b , G. Rusul a a Faculty of Food Science and Technology, Department of Food Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia b Faculty of Food Science and Technology, Department of Food Technology, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia a r t i c l e i n f o Article history: Received 19 May 2006 Received in revised form 29 January 2008 Accepted 19 March 2008 Keywords: Jackfruit volatile compounds Artocarpus heterophyllus L. Cultivars Fruit quality Fruit aroma Solid-phase microextraction Gas chromatography Time-of-ight mass spectrometry Principal component analysis Food composition Food analysis a b s t r a c t In the present study, the jackfruit volatile compounds were established using solid-phase microextrac- tion (SPME) and gas chromatography-time-of-ight mass spectrometry (GC-TOFMS). Qualitative and quantitative analyses were carried out using 5g samples with divinylbenzene/carboxen/polydimethyl- siloxane (DVB/CAR/PDMS) bre at 30 1C for 10 min. Rapid spectral acquisition rate of 10 spectra/s by the GC-TOFMS permitted identication and quantication of compounds having chromatographic peak widths of only a fraction of second. For SPME-GC-TOFMS analysis, the total time was approximately 18min. Thirty-seven compounds were identied from ve jackfruit cultivars. The main jackfruit volatile compounds were: ethyl isovalerate, 3-methylbutyl acetate, 1-butanol, propyl isovalerate, isobutyl isovalerate, 2-methylbutanol, and butyl isovalerate. These compounds were consistently present in all the ve cultivars and this suggests the compounds contributed to the sweet and fruity note of jackfruit. Principal component analysis (PCA) applied to the data, differentiated the ve jackfruit cultivars according to their unique avour compounds and explained 88% of the total variance. & 2008 Elsevier Inc. All rights reserved. 1. Introduction Because jackfruit (Artocarpus heterophyllus L.) is cross-pollinated and mostly seed propagated, it exhibits a wide range of variation in fruit quality. Different cultivated varieties vary widely in size, shape, bearing, and sensory qualities. Cultivars of commercially cultivated jackfruit are known with different local names (Nagy et al., 1990). Flavours are one of the most important components responsible for the nal overall distinctive sensory properties (i.e. taste and smell) in food. While the appearance and colour of a food provides the rst indication of quality, avour is critical in conrming that initial impression (Cardello, 1994). In the case of fruits, aroma is one of the most appreciated characteristics. Flavour is an important character- istic which can be used to distinguish different types of fruits or fruits belonging to the same variety but different cultivars (Kays, 1991). Fruit avour is particularly sensitive to compositional alterations. The volatiles produced by a harvested product can be altered by a wide range of preharvest and postharvest conditions. Overall, avour is affected by genetics, preharvest environment, harvest maturity, and postharvest handling or storage. Both qualitative and quantitative information are desired in order to monitor avour quality and ripeness and to provide quality control for fresh and processed products (Baldwin et al., 1999a; Romani et al., 1983; Fellman et al., 1993b). The most typically utilized methods for extraction and preconcentration are headspace techniques, purge and trap, liquidliquid extraction, simultaneous distillationextraction, solid-phase extraction, and supercritical uid extraction. Most of these methods are very time consuming and require exhaustive concentration steps. Solid-phase microextraction (SPME) is a solventless extraction alternative to conventional sample extrac- tion technique. In SPME, analytes establish equilibria among the sample matrix, the headspace above the sample, and a stationary phase coated on a fused silica bre; they are then thermally desorbed from the bre to a capillary column. SPME has been applied to the analysis of volatile and nonvolatile compounds (Arthur and Pawliszyn, 1990) in gaseous and liquid samples and to analyse avour in apple juice (Zierler et al., 2004), apple (Matich et al., 1996; Song et al., 1997), beef (Moon and Li-Chan, 2004), wine (Demyttenaere et al., 2003; Marti et al., 2003), cheese ARTICLE IN PRESS Contents lists available at ScienceDirect journal homepage: www.elsevier.com/locate/jfca Journal of Food Composition and Analysis 0889-1575/$ - see front matter & 2008 Elsevier Inc. All rights reserved. doi:10.1016/j.jfca.2008.03.002
E-mail address: nazimah@putra.upm.edu.my (S.A.H. Nazimah). Journal of Food Composition and Analysis 21 (2008) 416422 (Chin et al., 1996; Lecanu et al., 2002; Bellesia et al., 2003; Kim et al., 2003a), avocado (Lopez et al., 2004), and coffee (Bicchi et al., 2002; Akiyama et al., 2003). However, SPME application in analysing jackfruit avour of different cultivars has yet to be reported. Time-of-ight in a eld-free chamber is a measure of ion mass and is ideally suited for very rapid sampling rates, and it essentially detects all the ions in a mass spectrum simultaneously, instead of scanning the spectrum. This yields a large increase in the sensitivity with which product ion spectra are detected, up to 100-fold in favourable cases (Mellon et al., 2000). The speed of the detector is based on application of rapid gas chromatography (GC) separations with the resultant time compression of peaks. With the combination of fast GC and the time-of-ight mass spectro- meter (TOFMS), the quantitative and qualitative analysis time can be shortened at least 10-fold (Song et al., 1997). The aim of the present study was to (1) characterize the volatile compounds prole of ve jackfruit cultivars and (2) determine the major volatile compounds responsible for jackfruit avour by using principal component analysis (PCA). 2. Material and methods The solid-phase assembly holder and 65mm polydimethylsi- loxane (PDMS), 50/30mm divinylbenzene/carboxen/polydimethyl- siloxane (DVB/CAR/PDMS), and 65mm polydimethylsiloxane/ divinylbenzene (PDMS/DVB) were purchased from Supelco (Bellefonte, PA, USA). Standards were purchased from Aldrich Chemical Co. (Milwaukee, WI, USA) and Fluka Chemical Corp. (Buchs, Switzerland). 2.1. Plant material Five cultivars of jackfruit (J1, J3, J6, J30, and J31) were obtained from a commercial farm in Bidor, Perak, Malaysia. Three batches of fruits were collected at different harvesting periods (May, July, and August 2004). The harvested fruits were immediately transported on the same day to the laboratory at Universiti Putra Malaysia. Fruits were then allowed to ripen at ambient tempera- ture (7281C; 7075% RH) for 5 days. Fruits were cleaned and cut. The fruit bulbs were removed and deseeded prior to analysis. Fresh samples were randomly selected for avour analysis. Analyses were carried out in triplicates. 2.2. Standards and sample preparation For qualitative and quantitative analyses, standard mixtures were prepared by diluting methyl 3-methylbutanoate, ethyl 3-methylbutanoate, hexanal, propyl 3-methyl butanoate, 2-methylpropyl 3-methyl-butanoate and benzaldehyde with methanol to give a concentration ranging from 0.1 to 50ppm. Jackfruit pulp (100g) together with 500ppm propyl propanoate and methyl hexanoate in methanol dissolved as internal stan- dards, were homogenized using a Waring blender for 2min. The concentration of internal standard in the jackfruit sample was 5.0ppm. It should be noted that the addition of internal standard plus external standard has been basically recommended for quantitative analysis using SPME-GC in previous literatures (Pawliszyn, 1998; Supelco Bulletin 929, 2001). Five concentration levels of each analyte ranging from 0.1 to 50ppm were prepared for plotting standard calibration curves. For quantitative analysis, the [volatile compound/internal standard] peak area ratio obtained for each compound was interpolated into the calibration curves. In this study, 10ml of butyl acetate standard solution (1000mg l 1 ) was used as internal standard. A 5g sample was weighed into a 20 ml headspace vial, with Teon-lined septum was immediately sealed with an aluminium crimp seal. The headspace depth was approximately 4cm. 2.3. SPME sampling SPME bres were used to collect and concentrate volatiles by virtue of its sorption characteristics (Arthur and Pawliszyn, 1990). The bre is housed in a stainless-steel needle, which allows for penetration of the membrane covering the sample vial and the septum in the GC injection port. Once inside the sample vial, the bre was pushed out of the assembly holder and exposed to the headspace above the sample and equilibrated with the sample at 301C. The results obtained from our preliminary work indicated that the HS-SPME extraction at 301C for 10min using 5g sample with DVB/CAR/PDMS bre under stirring mode resulted in the largest extraction efciency. Samples were equilibrated at 30 1C for 30min prior to sampling (data not shown). Thus, the corresponded optimum condition was considered for qualitative and quantitative analyses in the present study. The SPME bre was then removed from the sample vial and volatiles adsorped onto the bre were thermally desorbed from the bre into the glass-lined, splitless-split injector port of a gas chromatography (Agilent 6890N) for 5min at 2501C. Each of the three bres was preconditioned at recommended temperature for a recommended time according to the manufacturers instruction. Samples were equilibrated at 301C for 30min prior to sampling. 2.4. Separation and detectionSPME/GC/TOFMS Absorbed volatiles were desorbed from the bre into the Agilent 6890 GC as described previously. Volatiles were separated using a capillary column (Supelco Wax-10, 10m0.1mm i.e. 0.1mm lm thickness). The ow rate of the carrier gas, heliumwas at a constant ow rate of 0.2ml min 1 . The temperature programme was isothermal for 1.5min at 401C and then raised at the rate of 251Cmin 1 2501C, and held for 1min. The GC/MS transfer line temperature was 2201C. Mass spectra were collected at a rate of 30 spectra/s over a range of m/z 35400. Volatiles were detected with TOFMS using electron ionization (LECO Pegasus 3; LECO Corporation, St. Joseph, MI). The ionization energy was 70eV. Data were analysed using the LECO deconvolution software (ChromTOF). Identication of volatile components was conrmed by matching the mass spectra obtained from authenticated standards and spectra in the National Institute of Standards and Technology (NIST) mass spectral library, Version 2.0. Quantica- tion was performed by external calibration and calibration curves were plotted on a series of concentration of the standards. 2.5. Statistical analysis Data collected was subjected to analysis of variance (ANOVA) using the MINITAB statistical software (Version 13, USA) and PCA (Unscrambler, Version 7.6, CAMO A/S, Trondheim, Norway). Analyses were performed on standardized mean data. Full cross- validation was used as a validation criterion. 3. Results and discussion 3.1. Selection of bre and extraction time For the selection of a suitable bre for adsorption of volatile compounds in the headspace of jackfruit samples, three types of ARTICLE IN PRESS B.T. Ong et al. / Journal of Food Composition and Analysis 21 (2008) 416422 417 SPME bres (i.e. 65mm PDMS, 65mm PDMS/DVB, and 50/30mm DVB/CAR/PDMS) were evaluated. Among the three SPME bres tested, 50/30mm DVB/CAR/PDMS bre coating showed better signal response than the two other bres for total peak area (Fig. 1). More compounds were also extracted using 50/30mm DVB/CAR/PDMS. Therefore, 50/30mm DVB/CAR/PDMS bre was selected in this study as the most suitable bre due to its high sensitivity with good reproducibility. The reproducibility of SPME bre was expressed as the coefcient of variation (RSD) on the peak areas of the volatile compounds after triplicate extraction. Low RSD% showed high reproducibility of headspace sampling. RSD for selected volatile compounds detected by all three bres was in the range of 25% (data not shown). PDMS coating has been used for analysis of both polar and non-polar volatile compounds (Miller et al., 1996; Steffen and Pawliszyn, 1996). According to Moon and Li-Chan (2004) this may be the result of improved stability of coating material as compared to other commercially available bres. The authors reported total area counts of the headspace volatiles of beef avour with a coefcient of variation of 2.9% and observed no signicant carry over from previous injection using the 50/30mm DVB/CAR/PDMS. According to Young et al. (1996) as cited by Keszler and He berger (1999), the average error in SPME method can be characterized by RSD that may range between 2.5% and 37%. In headspace SPME techniques, the extraction time is an important parameter inuencing the extraction yield. Fig. 2 shows that the extraction time of 10min using DVB/CAR/PDMS yielded the largest recovery of analytes. Signal response or peak area of the analytes increased signicantly (Po0.05) at 10min of extraction time. The response decreased at an extraction time of 15min, and reached a plateau at 30min. The point where the curve plateaus or levels off is considered to be the equilibration time (Steffen and Pawliszyn, 1996). Zierler et al. (2004) deter- mined off-avour compounds in apple juice and reported a similar behaviour where the recovery of the analytes decreased insignif- icantly with increasing extraction time and concluded that this behaviour may be possibly due to the saturation of the bre and beginning of the desorption processes. 3.2. Volatile compounds of jackfruit cultivars TOFMS was found to be of sufciently sensitivity for rapid and efcient detection of aroma volatiles. According to Song et al. (1997), the unskewed nature of fragmentation patterns obtained, allowed individual component spectral characterization of un- known compounds even when not fully chromatographically separated. Thus, the time required for chromatography could be reduced by an order of magnitude without loss in analytical performance. In this study, the determination of volatile com- pounds in jackfruit using SPME/GC-TOFMS was approximately 18min. ARTICLE IN PRESS 3.E+07 3.E+07 2.E+07 2.E+07 1.E+07 5.E+06 0.E+00 3 - m e t h y l b u t a n a l M e t h y l i s o v a l e r a t e E t h y l i s o v a l e r a t e B u t y l
a c e t a t e 3 - m e t h y l b u t y l a c e t a t e p r o y l i s o v a l e r a t e I s o b u t y l i s o v a l e r a t e 3 - m e t h y l b u t a n o l B u t y l i s o v a l e r a t e n - A m y l i s o v a l e r a t e Volatile compounds PDMS PDMS/DVB DVB/CAR/PDMS P e a k
A r e a Fig. 1. Comparison of different SPME bres (PDMS, PDMS/DVB and DVB/CAR/PDMS) after extraction for 10 min at 30 1C and separated using Supelco Wax-10 (10 m0.1mm i.e. 0.1mm lm thickness). 3.E+07 2.E+07 2.E+07 1.E+07 5.E+06 0.E+00 5 10 15 30 Extraction time (min) P e a k
A r e a 3-methylbutanal Butyl acetate Isolbutyl isovalerate n-Amyl isovalerate Methyl isovalerate 3-methylbutyl acetate 3-methylbutanol Ethyl isovalerate Proyl isovalerate Butyl isovalerate Fig. 2. Effect of extraction time at 301C on the extraction efciency of volatile compounds using DVB/CAR/PDMS bre. B.T. Ong et al. / Journal of Food Composition and Analysis 21 (2008) 416422 418 Five cultivars of jackfruit were analysed to determine qualita- tive and quantitative compositions of volatile compounds present in the fruit. Thirty-seven compounds were extracted from the ve different cultivars using the SPME method, including 20 esters, ve alcohols, nine aldehydes, two ketones, and one ether (Table 1). Using this method, 19 volatile compounds were detected in jackfruit. Eighteen of the volatile compounds detected were previously reported by Swords et al. (1978), Rasmussen (1983) and Maia et al. (2004). Among the 37 volatile compounds, which were mainly esters, the combinations in volatile compounds as well as their concentration were observed to be different in each cultivar (Table 1). However, several of the volatile compounds detected seemed to appear in all cultivars at relatively high concentrations. These volatile compounds were ethyl isovalerate, 3-methylbutyl acetate, 1-butanol, propyl isovalerate, isobutyl isovalerate, 2-methyl-1-butanol, and butyl isovalerate. Consistent occurrence of these compounds in all cultivars of jackfruit suggested its importance in contributing to the sweet and fruity note of jackfruit. Swords et al. (1978) detected butyl isovalerate, butyl butyrate, isoamyl isovalerate, butyl acetate, isobutyl isovalerate and propyl isovalerate in jackfruit distillates, and concluded that the mild oral aroma of jackfruit was due to the predominance of esters over aliphatic alcohols. The total absence of terpenoids was considered a unique feature of jackfruit. Cunningham et al. (1985) ARTICLE IN PRESS Table 1 Volatile compounds and their avour descriptors of ve jackfruit (Artocarpus heterophyllus L.) cultivars No Compounds Concentration (ppm) Odour descriptions J31 J1 J6 J30 J3 J4 1 Acetaldehyde 0.117 0.119 0.129 0.114 0.108 2 Acetone ND ND ND 0.112 0.108 Light ethereal, nauseating, fruity d 3 Methyl acetate 0.111 0.107 ND 0.106 ND Sweet, ethereal d 4 Butanal 0.124 0.110 ND 0.159 0.109 Pungent irritating d 5 Ethyl Acetate 0.125 0.109 0.112 0.109 0.109 Ethereal, banana-like, fruity d 6 2-Methylbutanal ND ND 0.115 ND ND Cocoa-like, coffee-like d , buttery, oily e 7 3-Methylbutanal 0.127 0.129 0.151 0.176 0.119 Pungent f , green, malty g , buttery, oily e 8 Ethanol 0.120 0.117 0.165 0.116 0.131 Alcohol, mild g , sweet d 9 n-Propyl acetate a 0.154 0.109 0.109 0.114 0.111 Ethereal, pear-like, raspberry-like d 10 2-Pentanone 0.109 ND ND 0.113 ND Sweet d , fruity, banana-like g 11 Isobutyl acetate 0.137 ND ND 0.111 ND 12 Methyl isovalerate a,b 0.132 0.133 0.363 0.388 0.231 Sweet, ethereal, apple-like, pineapple-like d 13 Ethyl butanoate a,b,c 0.108 0.123 0.127 0.107 0.117 Fruity, banana-, pineapple-like h 14 Propyl propanoate i.s i.s i.s i.s i.s. 15 2-Methyl-3-(methylthio)-butane ND ND ND 0.171 ND 16 Ethyl 2-methylbutanoate a ND ND 0.174 ND ND Apple-like, fruity, green h 17 Ethyl isovalerate a,b,c 0.358 0.261 0.986 0.238 0.937 Fruit odour reminiscent to apple i , fruity, berry j 18 Butyl acetate a,b,c 0.988 0.241 ND 0.509 0.455 19 Hexanal 0.028 0.024 0.033 0.029 0.022 20 2-Methyl-1-propanol b ND 0.055 ND ND ND Pungent, acid, fruity k 21 Tiglaldehyde ND 0.067 0.144 0.262 ND Pungent, green, ether, nutty, fruity l 22 2-Methylbutyl acetate a,c 3.692 ND ND ND ND Overripe fruit, sweet, banana-like, juicy fruit d 23 3-Methylbutyl acetate a,c 8.284 0.499 0.854 2.682 1.759 Fruity, pear-, banana-like d 24 1-Butanol b,c 0.721 0.359 0.395 0.513 0.429 Sweet d 25 Propyl isovalerate a,b,c 1.151 0.886 0.858 0.519 1.059 Fruity odour i 26 Pentyl acetate ND ND ND 0.308 ND Banana oil, fruit pineapple-like d 27 Methyl hexanoate i.s i.s i.s i.s i.s. 28 Isobutyl isovalerate a,b,c 0.754 0.775 0.730 0.430 0.586 Sweet, fruity, apple, raspberry, green k 29 2-Methyl-1-butanol b 0.794 0.558 0.906 0.630 0.469 Butter, fusel oil-like k , sweet, valeric d 30 3-Methyl-1-butanol b,c 1.753 1.215 1.591 1.163 0.711 Fruity, alcohol,whiskey g , rancid, pungent f 31 2-Hexenal ND ND ND 0.357 ND Grass-like, fruity, green d , apple-like m 32 Butyl butanoate a,b,c ND ND ND ND 0.390 Pear-, pineapple-like f , fresh, sweet, fruity d 33 Butyl isovalerate a,b,c 1.958 1.081 0.712 0.581 1.163 34 Isoamyl butanoate a,b ND 0.073 0.069 ND ND Sweet, apricot-, banana-like, fruity, oral d 35 Isoamyl isovalerate a,c ND 0.462 0.438 ND ND Sweet, fruity, fresh, ripe apple k 36 Hexyl acetate a,c ND ND ND 0.042 ND Fruity, oral d , sweet, berry-, pear-like h 37 n-Amyl isovalerate 1.166 0.503 ND 0.124 0.451 38 Benzaldehyde ND 0.045 0.157 ND 0.052 Strong, sweet, bitter almond, cherry d 39 Benzenepropanal ND ND 0.131 ND ND J31, J1, J6, J30 and J3 using DVB/CAR/PDMS ber. ND not detected. a Maia et al. (2004). b Rasmussen (1983). c Swords et al. (1978). d Shibamoto and Tang (1990). e Akiyama et al. (2003). f Jorda n et al. (2001b). g Lecanu et al. (2002). h Takeoka et al. (1989). i Burdock (2002). j Marti et al. (2003). k Anon (2002). l Paillard (1990). m Kim et al. (2003b). B.T. Ong et al. / Journal of Food Composition and Analysis 21 (2008) 416422 419 studied the aroma components in 40 cultivars of apple and found that apple aroma was not the result of the same compounds in every cultivar, although some common volatile compounds were important in all cultivars. Using PCA, volatile compounds detected can be grouped and related statistically to each cultivar as shown in Fig. 3. Correlation matrices were computed and three principal components (PC1, PC2, and PC3) explained 88% of the total variance. Bi-plots (Figs. 3 and 4) revealed that PC1 and PC2 explained 41% and 27% of the total variation. The volatile compounds detected were clearly clustered into its ve jackfruit cultivars (cultivars J1, J31, J3, J6, and J30) as shown in Fig. 3. Further evaluation of the cultivars avour by sensorial descriptive analysis and olfatometric evaluation of volatile compounds isolated by SPME method are recommended and will enable deeper understanding of the characteristic aroma that contribute to the avour of each jackfruit cultivar. Propyl isovalerate, isobutyl isovalerate, isoamyl butanoate, and isoamyl isovalerate, which lie in the negative region of PC1 and positive region of PC2 were clustered together with cultivar J1. These compounds were present at concentration of 0.886, 0.775, 0.073, and 0.462ppm, respectively, and were relatively higher compared to the concentration in other cultivars. These com- pounds are reported to produce an aroma which is sweet in mixtures of apple-, banana- and raspberry-like fruity odour (Swords et al., 1978; Rasmussen, 1983; Maia et al., 2004). Another unique compound detected is 2-methyl-1-propanol (0.055ppm), the odour of which according to Shibamoto and Tang (1990) as pungent, acid and fruity. Several other volatile compounds, which lie on the positive regions of PC1 and PC2, were correlated with cultivar J31 (Fig. 3). Methyl acetate, ethyl acetate, n-propyl acetate, 3-methylbutyl acetate, 1-butanol and 3-methyl-1-butanol were present at a concentration of 0.111, 0.125, 0.154, 8.284, 0.721, and 1.753ppm, respectively (Table 1). Their concentration in J31 was higher compared to other cultivars. 3-Methylbutyl acetate was detected in all the cultivars. The unique compound identied in cultivar J31 was 2-methylbutyl acetate at a concentration of 3.692ppm. Higher concentrations of 3-methylbutyl acetate and 2-methylbu- tyl acetate may contribute to a banana-like odour (Shibamoto and Tang, 1990). As shown in Fig. 3, both cultivars J3 and J6, and their characteristic compounds were clustered together. Principal component 3, which explained 20% of the total variance, clearly differentiated cultivar J3 from cultivar J6 (Fig. 4). Ethyl isovalerate (0.937ppm), ethyl butanoate (0.117ppm), butyl butanoate (0.390ppm), and ethanol (0.131ppm) were clustered with cultivar J3 at the positive region of PC3. These compounds have been described as sweet and fruity with pineapple-like odour (Shibamoto and Tang, 1990; Paillard, 1990). Occurrence of these compounds was also reported in apples, pears, quinces (Paillard, 1990) and other tropical fruits (Shibamoto and Tang, 1990). The cluster of volatile compounds for fruits of cultivar J6 was located near the origin of PC3 and could not be explained. However, with reference to Fig. 3 and Table 1, the volatile compounds were: 2-methylbutanal (0.115ppm), ethyl 2-methyl- butanoate (0.174ppm), and benzenepropanal (0.131ppm). These compounds were identied in the cultivar, J6. The presence of ethyl 2-methylbutanoate, which has an odour threshold of only 0.1ppb, may contribute to the fruity apple-like odour (Rowe, 2002). In Fig. 4, it can be clearly seen that compounds which completely differentiated cultivar J6 from cultivar J3 were benzaldehyde (0.157ppm) (Table 1) and propyl isovalerate. Benzaldehyde was also detected in some of the cultivars but its concentration in cultivar J6 was threefold higher. The occurrence of 2-methylbutanal, benzenepropanal and benzaldehyde may contribute to sharp, almond- and cocoa-like odour and when present may produce an odour that may not be acceptable by consumers (Shibamoto and Tang, 1990). ARTICLE IN PRESS -1.0 -0.5 0 0.5 1.0 1.0 0.5 0 -0.5 -1.0 J31 J1 J6 J30 J3 Acetal Acetone Met_ Acet But_al Et_Acet 2-Met-But_al 3-Met-But_al Et_oh n-Pro_acet 2-Pentanone 2-Met_pro_Acet Met_3mb Et_But 2-met-3-(methyl Et_2mb Et_3mb Butyl_Acet Hex 2-met-1-Propano E-2-Met-2-buten 2-Met_Butyl_Ace 3-Met_Butyl_Ace 1-Butanol Propyl-3mb Pentyl_Acet 2-MetPropyl-3mb 2-Met-1-Butanol 3-Met-1-Butanol 2-Hexenal Butyl_But Butyl-3mb 3-metbutyl_But 3-metbutyl-3mb Hexyl_Acet n-Amyl iso Benzal Benzenepropanal PC1 t o l p - i B P C 2 Fig. 3. Bi-plots of principal components 1 and 2 of the volatile compounds of ve jackfruit cultivars. Acetal: acetaldehyde; acetone; Met_Acet: methyl acetate; But_al: butanal; Et_Acet: ethyl acetate; 2-met_But_al: 2-methylbutanal; 3-Met-But_al: 3-methylbutanal; Et_oh: ethanol; n-Propyl_Acet: n-propyl acetate; 2-pentanone; Iso_Butyl Ace: isobutyl acetate; Met_iso: methyl isovalerate; Et_But: ethyl butanoate; Propyl_propano: propyl propanoate; 2-met-3-(met_thio)-But: 2-methy-3-(methylthio)-butane; E-2-Met_But: ethyl 2-methylbutanoate; Et_iso: ethyl isovalerate; Butyl_Ace: Butyl acetate; Hexanal; 2-met-1-propanol: 2-methyl-1-propanol; Tiglal: tiglaldehyde; 2-Met_Butyl_Ace: 2-methylbutyl acetate; 3-Met_Butyl_Ace: 3-methylbutyl acetate; 1-butanol; Propyl_iso: propyl isovalerate; Pentyl_Ace: pentyl acetate; Met_ hex: methyl hexanoate; Iso_Butyl_iso: isobutyl isovalerate; 2-Met-1-Butanol: 2-methyl-1-butanol; 3-Met-2-Hex_al: 3-methyl-2-hexenal; Butyl_But: butyl butanoate; Butyl_iso: butyl isovalerate; Iso_but: isoamyl butanoate; Isoamyl_iso: isoamyl isovalerate; Hex_Ace: hexyl acetate; n-Amyl iso: n-amyl isovalerate; Benzal: benzaldehyde; Benzenepropanal. B.T. Ong et al. / Journal of Food Composition and Analysis 21 (2008) 416422 420 Finally, fruits of cultivar J30 (Fig. 3 and Table 1) contained acetone (0.112ppm), butanal (0.159ppm), 3-methylbutanal (0.176ppm), 2-pentanone (0.113ppm), methyl isovalerate (0.388ppm), and tigaldehyde (0.262ppm). In addition, cultivar J30 has four other unique compounds, namely 2-methyl- 3-(methylthio) butane (0.171ppm), pentyl acetate (0.308ppm), 2-hexenal (0.357ppm) and hexyl acetate (0.042ppm), which were not found in other cultivars. A combination of these characteristic compounds may indicate a avour note of fruity apple- and pineapple-like odour along with strong, pungent, nauseating, irritating, and green odour (Shibamoto and Tang, 1990; Paillard, 1990; Jordan et al., 2001a, b; Lecanu et al., 2002; Akiyama et al., 2003; Kim et al., 2003b). The volatile compounds clustered in both cultivars J1 and J31, which lie on the positive region of PC2, are the most common volatile compounds in jackfruit avour. On the other hand, jackfruit avour of cultivars J3, J6, and J30 were located at the negative region of PC2. A mixture of different combinations and concentrations of volatile compounds is the main factor which gives the unique avour of each cultivar tested. 4. Conclusion SPME is a rapid extraction method with high reproducibility in food avour analysis. TOFMS provided sufcient sensitivity and speed to permit rapid and efcient detection of aroma volatiles. Volatile compounds determined in this study were predominantly esters and may respond to the unique avour and aroma of jackfruit. Therefore, quantication of the concentration of volatile compounds present plays an important role in determining the effect of the compounds in the overall avour of the fruit in each cultivar. Besides, each cultivar had its own unique compound which differentiated them from one to another. Majority of the volatile compounds which differentiated each cultivar were present in higher concentration. PCA was found useful in grouping the volatile compounds according to its cultivar. Acknowledgement Special thanks and gratitude to University Putra Malaysia for providing the research Grant IRPA 01-02-04-0789 EA001 that enable the authors to carry out the work. References Anon, 2002. Honey, smell this. Is it bad? Food Quality 34, 3639. Akiyama, M., Murakami, K., Ohtani, N., Iwatsuki, K., Sotoyama, K., Wada, A., Tokuno, K., Iwabuchi, H., Tanaka, K., 2003. Analysis of volatile compounds released during the grinding of roasted coffee beans using solid-phase microextraction. Journal of Agricultural and Food Chemistry 51, 19611969. Arthur, C.L., Pawliszyn, J., 1990. Solid phase microextraction with thermal desorption using silica optical bers. Analytical Chemistry 62, 21452148. 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Acetal: acetaldehyde; acetone; Met_Acet: methyl acetate; But_al: butanal; Et_Acet: ethyl acetate; 2-met_But_al: 2-methylbutanal; 3-Met-But_al: 3-methylbutanal; Et_oh: ethanol; n-Propyl_Acet: n-propyl acetate; 2-pentanone; Iso_Butyl Ace: isobutyl acetate; Met_iso: methyl isovalerate; Et_But: ethyl butanoate; Propyl_propano: Propyl propanoate; 2-met-3-(met_thio)-But: 2-methyl-3-(methylthio)- butane; E-2-Met_But: ethyl 2-methylbutanoate; Et_iso: ethyl isovalerate; Butyl_Ace: butyl acetate; Hexanal; 2-met-1-propanol: 2-methyl-1-propanol; Tiglal: tiglaldehyde; 2-Met_Butyl_Ace: 2-methylbutyl acetate; 3-Met_Butyl_Ace: 3methylbutyl acetate; 1-Butanol; Propyl_iso: propyl isovalerate; Pentyl_Ace: pentyl acetate; Met_ hex: methyl hexanoate; Iso_Butyl_iso: isobutyl isovalerate; 2-Met-1-Butanol: 2-methyl-1-butanol; 3-Met-2-Hex_al: 3-methyl-2-hexenal; Butyl_But: butyl butanoate; Butyl_iso: butyl isovalerate; Iso_but: isoamyl butanoate; Isoamyl_iso: isoamyl isovalerate; Hex_Ace: hexyl acetate; n-Amyl iso: n-amyl isovalerate; Benzal: benzaldehyde; Benzenepropanal. 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