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Volatile profile of yellow passion fruit juice by static headspace and solid phase microextraction techniques/Perfil volatil do suco do maracuja-amarelo por tecnicas de extracao em headspace estatico e microextracao em fase solida.


The yellow passion fruit (Passiflora edulis f. flavicarpa Deg.) is the most widely cultivated Passiflora species in Brazil and much appreciated by the intense aroma and taste of its juice. The chemical composition of yellow passion fruit juice is characterized by the presence of volatile and non-volatile substances, which define their sensory and nutritional attributes. In the case of volatile compounds, they interfere directly with the sensory quality of the fruit and its processed products (PONTES et al., 2009). The juice of yellow passion fruit has an "ester" floral aroma with exotic tropical characteristic of sulfurous note (CARASEK & PAWLISZYN, 2006). Notably, volatiles aroma of fruits are composed of a complex group of chemical substances, such as aldehydes, alcohols, ketones, esters, lactones and terpenes (JORDAN et al., 2002). However, terpenes and esters are more related to the aroma of passion fruit juice (MACORIS et al., 2011). Additionally, the major volatile compounds identified in yellow passion fruit juice belong to the methyl and ethyl esters (WERKHOFF et al., 1998; CARASEK & PAWLISZYN, 2006). The levels of individual volatile compounds related to the aroma profile in food matrix are largely influenced by the extraction technique of the volatile fraction used in gas chromatograph analysis (BICCHI et al., 2008). Headspace sampling techniques are widely used for providing volatile profiles near the profiles experienced by humans. Based on the collection of the volatile compounds in the gaseous phase above, a sample under defined conditions is dependent on the volatility of the aromatic compounds (GUTH & GROSCH, 1993). Among the headspace techniques currently used for the extraction of aromatic volatiles, solid-phase microextraction (HS-SPME) has been applied for isolation of volatile compounds from fruits (BARBONI et al., 2009; PONTES et al., 2009; FIGOLI et al., 2010, ALVAREZet al., 2012). This technique is based on a dynamic process of adsorption ofvolatiles on the vapor phase in the sample headspace in a silica fiber coated with an adsorbent polymer and has high sensitivity in the volatiles extraction with a wide range of polarity (BICCHI et al. 2008). In the static headspace sampling techniques (S-HS), the equilibrium between the sample and the headspace gas phase must be reached, and a gaseous fraction of the headspace is collected directly for analysis by gas chromatograph (SNOW & SLACK, 2002; WANG et al., 2008). The S-HS technique is simpler and faster and has been used in comparative analysis of the flavor profile of vegetable matrices (MILLER & STUART, 1999; VARMING et al., 2004; BYLAITE &MEYER, 2006; UBEDA et al. 2011). However, S-HS has not yet been used in the analysis of yellow passion fruit juice volatiles. The S-HS procedure is free of solvents, demands little sample handling, and can be automated, but its sensitivity is considered low compared to SPME, being indicated for the analysis of compounds whose boiling points are low (MESTRES et al., 2002). Nevertheless, the S-HS sensitivity can be increased by salt addition, pH control or increasing the equilibrium temperature during sample heating (B'HYMER, 2003), which can improve the recovery of major volatile compounds of the aroma of passion fruit, such as esters and terpenes. Therefore, the aim of this study was to determine the profile of volatile compounds of the yellow passion fruit juice through the headspace solid-phase microextraction (HS-SPME) and optimized static headspace (S-HS) extraction techniques.


Yellow passion fruits were harvested in April 2011 in an orchard in Piracicaba, Sao Paulo State, Brazil, located at 22043'31" south latitude and 47[degrees]38'57'' west longitude. Fruits were selected on the yellow-ripe physiological stage, healthy and without physical defects. For assays, 15 fruits were chosen with lengths between 8 and 10cm. A cross section was made in each fruit to extract the pulp (juice and seed). The juice was separated from the seed by drainage through a plastic sieve and then was frozen and stored at -24[degrees]C until the time of analysis. The frozen juice samples were first thawed in water bath at 25[degrees]C for analyses on HS-SPME and S-HS. The extractions were performed without pH adjustment. All analyzes were performed in triplicate. For the extraction in HS-SPME, the equilibrium parameters were established according to PONTES et al. (2009) with modifications. In a 20mL flask 0.2mL aliquot of juice sample was diluted with 1.0mL Milli-Q water (Millipore Corporation, Brazil). The solution ionic strength was increased to improve the extraction efficiency with the addition of 17% NaCl (0.2g, [wv.sup.-1]) in the diluted sample. The vial was tightly sealed with a screw cap with coupled silicone septum. The fiber used in the HS-SPME extraction had the coating of polydimethylsiloxane/divinylbenzene (PDMS / DVB, Supelco Inc., Bellefonte, PA, USA). The fiber was exposed in the sample headspace and maintained for 20 minutes at 50[degrees]C, with the sample in a thermostatic magnetic stirrer at 450rpm. After the extraction procedure by adsorption in the headspace, the fiber was inserted into the injector of the gas chromatograph-mass spectrometry system for 6 minutes in the splitless mode, where the extracted volatiles were thermally desorbed at 250[degrees]C.

In the S-HS technique the parameters of equilibrium between gas and liquid phases of the passion fruit sample were adjusted to improve the extraction efficiency with higher recovery levels and volatile concentration as possible. The time and temperature, sample volume and the NaCl concentration were considered as equilibrium parameters in the gas phase of the sample. The NaCl concentration was adjusted by adding 10, 20 and 30% ([wv.sup.-1]) salt and the control without salt. The NaCl addition in the sample decreases the solubility of volatile compounds, increasing its volatility in the sample (PONTES et al., 2009). The optimal salt concentration was established keeping invariable the conditions of time and equilibrium temperature in 20 minutes and 70[degrees]C. Times of 10, 20 and 30 minutes and temperatures of 50, 60, 70, 80 and 90[degrees]C were tested. Above 90[degrees]C the sample reached the boiling point and therefore was chosen as the limit temperature. The choice of best time of equilibrium was carried out at the temperature of 60[degrees]C. The selection of the binomial time and temperature of equilibrium was achieved with the addition of the best NaCl concentration adjusted (w v-1) in the juice sample. The adjusted condition of equilibrium in the headspace for temperature and time was used for adjusting the sample volume with 2.5, 5.0 and 7.5mL. The heating of the juice sample at all procedures for balance adjustment in the headspace occurred under constant stirring in a glass flask silalized (20mL) and hermetically sealed with a screw cap with a coupled silicone septum. The volume of 1.5mL was collected from the headspace and injected into the gas chromatograph with Shimadzu automatic injector equipped with heating oven of the sample.

The volatile compounds sampled in S-HS and HS-SPME were analyzed in a gas chromatograph Shimadzu 2010 coupled to a mass spectral detector Shimadzu QP 2010 Plus. The samples were separated in DB5 capillary column (30mx0.25mm x0.25[micro]m, J&W Scientific, Palo Alto, CA). Mass spectra and total ion currents (TIC chromatograms) were obtained by automatic scanning with energy ionization 70 eV, in the mass range m/z 35-500. The temperature ramp began at 40[degrees]C maintained for 4.0min, then 150[degrees]C at 3.0[degrees]C [min.sup.-1] and 250[degrees]C at 15[degrees]C [min.sup.-1] maintained for 2.0 min. Helium was used as carrier gas at linear velocity of 36.1cm [s.sup.-1]. Kovats indices of linear retention (KI) of the chromatographic peaks obtained were determined experimentally based on the retention time of a homologous n-alkanes series (C6-C18).

Peaks were tentatively identified based on: I) comparison of fragmentation patterns using the mass spectral database of the library Wiley8 of the GCMSsolution Software identification system (Mass Spectrometer Systems--Shimadzu) II) by comparing the Kovats retention indices (KI) obtained experimentally with theoretical ratios obtained from the literature. The compounds were expressed as relative amounts to the peak areas percentage.

The Analysis of variance was used to check for significant differences in tests of headspace balance adjustment and among the methods of volatiles extraction. The significance level P<0.05 was considered. The statistical package SAEG (UFV --Vicosa, MG, Brazil) was used.


HS-SPME and S-HS are are simple, rapid, solvent-free extraction techniques and can help to analyze the volatile profile of vegetable matrices that have intense aroma to human scent, as the case of the yellow passion fruit juice. The temperature is a key parameter in the extraction yield and, with time, have a significant effect on the balance of the gas phase in the sample headspace, since they determine the vapor pressure of volatiles (CARASEK & PAWLISZYN, 2006), and for this reason, adjustments were made. In addition, the NaCl concentration and volume of juice samples were also adjusted. The results of these assays are shown in figure 1. There were significant increases (P<0.05) in total area of peaks with increasing equilibrium time in the range of 10 to 30min (Figure 1a), but between 20 and 30 min there were no significant differences among peak areas. Thus, the time of 20 min was selected because it was the shortest not significant contrast time. While adjusting the equilibrium temperature, the extraction time of 20min was maintained constant at all temperatures tested. According to figure 1b, increases in peak area values show that the extraction efficiency increased significantly (P<0.01) with increasing equilibrium temperature and the maximum extraction efficiency was achieved at 90[degrees]C. Preliminary analysis of the chromatographic peaks for the sample at 50, 60 and 90[degrees]C (not reported) showed no degradation of the volatiles in the sampling conditions at 90[degrees]C for 20 minutes.

No significant differences were found for the results of the total area when different NaCl concentrations were tested in the yellow passion fruit juice (Figure 1c), showing that the use of salt (NaCl) is not recommended in whole juice samples of yellow passion fruit by adding no increase efficiency in the extraction of volatiles in the S-HS technique. The NaCl addition in the sample aims to improve the extraction efficiency by increasing the ionic strength and decrease the solubility of volatile compounds soluble in the aqueous phase (PONTES et al., 2009). Probably, there was no effect of salt addition, since the ionic strength in the juice sample should be sufficiently high, justifying the high volatility of the volatile compounds of the yellow passion fruit. According to figure 1d, increasing the volume of juice influenced in significant increases (P<0.01) in the total area values of volatiles peaks, showing that the most efficient extraction of volatiles was achieved in 7.5mL juice sample and therefore, it was the chosen volume. Thus, the adjusted conditions of headspace equilibrium in the volatiles extraction in the S-HS technique were 90[degrees]C for 20min, 7.5mL sample volume for the juice without NaCl addition.

The results of yellow passion fruit volatile profiles obtained through S-HS and HS-SPME extraction techniques are shown in table 1. Kovats retention linear indices (KI) were calculated for each peak and, when evaluable, they were compared with the reference literatures in order to ensure the compounds identification. The percentage of total area for the S-HS and HSSPME extraction techniques were 96.85[+ or -]1.59% and 93.58[+ or -]1.25%, respectively. The differences in the total percentages (100%) represent the peak areas of the volatiles that have not had their identity confirmed by comparisons of mass spectra and Kovats linear retention indices (KI).

Among the different types of fibers routinely used for sampling of volatiles, which have a range of polarities and different mechanisms of selectivity, the PDMS/DVB fiber (polydimethylsiloxane/ divinylbenzene) was used in this study and the conditions of headspace equilibrium in the extraction with the fiber had been pre-established. The equilibrium conditions were extraction temperature of 50[degrees]C, extraction time of 20min, stirring at 450rpm and the addition of 17% NaCl([wv.sup.-1]). In a comparative study between five types of fibers it was observed that PDMS/DVB fiber was the most efficient for volatiles extraction in a sample of purple passion fruit juice (PONTES et al., 2009). These authors also found a high affinity of this fiber for ethyl esters, alcohols and terpenes.

According to table 1, analysis of the volatile profile of passion fruit juice (P edulis f. Flavicarpa Deg.) in GC/MS by the S-HS and HS-SPME techniques resulted in 30 and 44 identified volatile compounds, respectively. Esters, terpenes, alcohols, aldehydes and ketones formed the groups of volatiles identified in the study of yellow passion fruit and they probably play an important role in the juice sensory profile (WERKHOFF et al., 1998; MACORIS et al., 2011). In the HS-SPME technique recovery of volatiles was more efficient with the identification of 24 esters, 8 terpenes, 6 alcohols, 3 aldehydes, 2 ketones and one acid, while in S-HS extraction were identified 19 esters, 8 terpenes and 3 alcohols, not being identified in this extraction procedure the volatiles ketone and aldehyde groups. Among the esters identified in both extraction techniques, ethyl butanoate, ethyl hexanoate, (3z)-3-hexenyl acetate, hexyl acetate, hexyl butanoate and hexyl hexanoate were the major ones. However, similarities in area percentage among the esters identified in S-HS and HS-SPME were found only for (3Z)-3-hexenyl acetate (5.16%[+ or -]0.10 and 6.23[+ or -]0.12% respectively), hexyl acetate (7.96[+ or -]0.06% and 6:51[+ or -]0.63%, respectively) and hexyl butanoate (9.75[+ or -]0.10% and 11.88[+ or -]0.14% respectively), while the greatest differences were found for ethyl butanoate (16.86[+ or -]0.32% and 3.42[+ or -]0.63% respectively), ethyl hexanoate (21:15[+ or -]0.29% and 11.11[+ or -]1.08%, respectively) and hexyl hexanoate (9.49[+ or -]0.74% and 17.47[+ or -]1.33%, respectively).

According to reports in scientific study,volatile esters are the major compounds with the highest concentration of yellow passion fruit juice(JORDAN et al.,2002; CARASEK & PAWLISZYN, 2006). In addition,hexyl hexanoate, hexyl butanoate, ethyl butanoate, (Z)-3-hexenyl hexanoate, (Z)-3-hexenyl butanoate and ethyl hexanoate are the most abundant compounds found among the volatile fraction of yellow passion fruit juice (WERKHOFF et al., 1998; BRAT et al., 2000). In the present study, these compounds were identified in the two extraction techniques. Using dynamic headspace MACORIS et al. (2011) found ethyl butanoate in both organic and conventional passion fruit pulps produced in Brazil, with 52%and 57% of the total relative area of the chromatogram, respectively. Meantime, in the present study this specific compound was found in high concentrations only when the HS technique was used. However, the esters (Z)-3-hexenyl hexanoate and (Z)-3-hexenyl butanoate showed significant higher concentrations in HS-SPME extraction with area percentages of 6.48[+ or -] 0.34% and 3.26[+ or -]0.05% respectively, while in S-HS were found areas of 1.74[+ or -]0.19% and 1.62[+ or -]0.03%, respectively. Only esters butyl acetate and 2-ethyl hexanoate were not identified in HS-SPME; however, benzyl acetate, ethyl 3-octenoate, hexyl pentanoate, 1-pentyl-2-propenyl butanoate, 4-oxocyclohexyl acetate, and ethyl decanoate ethyl cinnamate were not identified in the S-HSprocedure.

Studies on volatile profile in Passiflora species with extraction procedures in HS-SPME (PDMS/DVB) showed 24 volatile compounds in the yellow passion fruit juice, and the most abundant esters were the methyl hexanoate (32.9%), followed by (E)-methyl-2-hexenoate (11.7%), methyl benzoate (11.3%), methyl dihydrojasmonate (6.2%)(PONTES et al., 2009). However, no volatile methyl esters were found in this study (Table 1).

Terpenes simultaneously identified in both extraction methods were [beta]-pinene, [rho]-cimene, limonene, (Z)-[beta]-ocimene, (E)-[beta]-ocimene, [gamma]-terpinene, [alpha]-terpinolene and (E)-4,8-dimethyl1,3,7-nonatriene. The largest sum of percentages of peak area for terpenes volatile found for the S-HSprocedure with 19.57[+ or -]1.19%, while in HS-SPME was found 11.94[+ or -]0.31%.Although with lower total intensity of peaks, terpenoids recovered in S-HS are the same recovered in HS-SPME, showing similarity extraction of terpenes volatile compounds. The similarity in the recovery of terpenes in both extraction techniques shows that these compounds, although not showing the highest concentration, present easily volatile in the fraction of passion fruit juice in comparison with some volatile esters and alcohols, and all aldehydes and ketones which were not identified in the S-HSprocedure. Hexanol, octanol and linalool were the only alcohols extracted and identified simultaneously in S-HS and HS-SPME. Other threealcohols 4-terpineol, (Z)-3,7-dimethyl-2,6-octadien-1-ol and decan-1-ol were identified only in the HS-SPME procedure. In addition to lower extraction efficiency to some esters and alcohols, S-HS procedure was not sensitive to recover volatile ketone and aldehyde groups (Table 1).


This study showed that the S-HS optimized extraction technique was effective to recovery high concentrations of characteristics major volatile compounds in the passion fruit, such as ethyl butanoate and ethyl hexanoate, which can be advantageous due to the simplicity of the method.[beta]-Pinene, p-cymene, limonene, (Z)-[beta]-ocimene, (E)[beta]-ocimene, [gamma]-terpinene, [alpha]-terpinolene and (E) -4,8-dimethyl-1, 3,7--nonatriene terpenes were identified with the same similarity of recovery in both techniques. This is important, because together these compounds are considered to be the most important for the characteristic passion fruit flavor.


The authors acknowledge to the Department of AgriFood Industry, Food and Nutrition/ESALQ/USP for the research infrastructure provided.


ALVAREZ, R. et al. Citrus juice extraction systems: effect on chemical composition andantioxidant activity of clementine juice. Journal of Agricultural and Food Chemistry, v.60, p.774-781, 2012. Disponivel em: <>. Acesso em: 15 fev. 2013. Doi 10.1021/jf203353h.

B'HYMER, C. Residual solvent testing: a review of gaschromatographic and alternative techniques. Pharmaceutical research, v.20, p.337-344, 2003. Disponivel em: < 6b54547eb7b5c1a43bf2&ext=.pdf>. Acesso em: 23 mar. 2013. Doi 10.1023/A:1022693516409.

BARBONI, T. et al. Volatile composition of hybrids Citrus juices by headspace solid-phase micro extraction/gas chromatography/mass spectrometry. Food Chemistry, v. 116, p.382-390, 2009. Disponivel em: <>. Acesso em: 24 mar. 2013. Doi 10.1016/j.foodchem.2009.02.031.

BICCHI C. et al. Headspace sampling of the volatile fraction of vegetable matrices. Journal of Chromatography A, v. 1184, p.220-233, 2008. Disponivel em: <>. Acesso em: 24 mar. 2013. Doi 10.1016/j. chroma.2007.06.019.

BRAT, P. et al. Free volatile components of passion fruit puree obtained by flash vacuum-expansion. Journal of Agricultural and Food Chemistry, v.48, p.6210-6214, 2000. Disponivel em: <>. Acesso em: 24 mar. 2013. Doi 10.1021/jf000645i.

BYLAITE, E.; MEYER, A.S. Characterization of volatile aroma compounds of orange juices by three dynamic and static headspace gas chromatography techniques. European Food Research and Technology, v.222, p.176-184, 2006. Disponivel em: <>. Acesso em 23 nov. 2012. Doi 10.1007/s00217-005-0141-8.

CARASEK, E.; PAWLISZYN, J. Screening of tropical fruit volatile compounds using solid-phase micro extraction (SPME) fibers and internally cooled SPME fiber. Journal of Agricultural and Food Chemistry, v.54, p.8688-8696, 2006. Disponivel em: <>. Acesso em 20 nov. 2012. Doi 10.1021/jf0613942.

DU, X. et al. Evaluation of volatiles from two subtropical strawberry cultivars using GC-olfactometry, GC-MS odor activity values, and sensory analysis. Journal of Agricultural and Food Chemistry, v.59, n.23, p.12569-12577, 2011. Disponivel em: <>. Acesso em: 17 out. 2012. Doi 10.1021/jf2030924

FIGOLI, A. et al. Evaluation of pervaporation process of kiwifruit juice by spme-gc/iontrap mass spectrometry. Desalination, v.250, p.1113-1117, 2010. Disponivel em: <>. Acesso em 20 nov. 2012. Doi 10.1016/j. desal.2009.09.120.

GUTH, H.; GROSCH, W. Identification of potent odourants in static headspace samples of green and black tea powders on the basis of aroma extract dilution analysis (AEDA). Flavour and Fragrance Journal, v.8, p. 173-178, 1993. Disponivel em: <>. Acesso em 17 out. 2012. Doi 10.1002/ffj.2730080402.

JORDAN, M.J. et al. Characterization of the aromatic profile in aqueous essence and fruit juice of yellow passion fruit (Passiflora edulis Sims F. Flavicarpa Degner) by GC-MS and GC/O. Journal of Agricultural and Food Chemistry, v.50, p.1523-1528, 2002. Disponivel em: <>. Acesso em 12 out. 2012. Doi 10.1021/jf011077p.

MACORIS, M.S. et al. Volatile compounds from organic and conventional passion fruit (Passiflora edulis F. Flavicarpa) pulp. Ciencia e Tecnologia de Alimentos, v.31, n.2, p.430435, 2011. Disponivel em: <>. Acesso em 20 nov. 2012. Doi 10.1590/ S0101-20612011000200023.

MAHATTANATAWEE, K. et al. Comparison of three lychee cultivar odor profiles using gas chromatography-olfactometry and gas chromatography-sulfur detection. Journal of Agricultural and Food Chemistry, v.55, n.5, p.1939-1944, 2007. Disponivel em: <>. Acesso em 12 nov. 2012. Doi 10.1021/jf062925p.

MESTRES, M. et al. Application of headspace solid-phase microextraction to the determination of sulphur compounds with low volatility in wines. Journal of Chromatography A, v.945, n.1-2, p.211-219, 2002. Disponivel em: <>. Acesso em 08 fev. 2013. Doi 10.1016/ S0021-9673(01)01521-7.

MILLER, M.E.; STUART, J.D. Comparison of gas-sampled and spme-sampled static headspace for the determination of volatile flavor components. Analytical Chemistry, v.71, p.23-27, 1999. Disponivel em: <>. Acesso em 15 out. 2012. Doi 10.1021/ac980576v.

PONTES, M. et al. Headspace solid-phase microextraction-gas chromatography-quadrupole mass spectrometric methodology for the establishment of the volatile composition of Passiflora fruit species. Microchemical Journal, v.93, p.1-11, 2009. Disponivel em: <>. Acesso em 15 out. 2012. Doi 10.1016/j.microc.2009.03.010.

RODRIGUEZ-BURRUEZO, A. et al. Comparative analysis of genotypic diversity in the volatile fraction and aroma-contributing compounds of Capsicum fruits from the annuumchinense-frutescen complex. Journal of Agricultural and Food Chemistry, v.58, n.7, p.4388-4400, 2010. Disponivel em: <>. Acesso em 16 out. 2012. Doi 10.1021/jf903931t.

SNOW, N.H.; SLACK, G.C. Head-space analysis in modern gas chromatography. Trends in Analytical Chemistry, v.21, p.608617, 2002. Disponivel em: <>. Acesso em 16 out. 2012. Doi 10.1016/S01659936(02)00802-6.

UBEDA, C. et al. Determination of major volatile compounds during the production of fruit vinegars by static headspace gas chromatography-mass spectrometry method. Food Research International, v.44, p.259-268, 2011. Disponivel em: <>. Acesso em 16 out. 2012. Doi 10.1016/j.foodres.2010.10.025.

VARMING, C. et al. Comparison of isolation methods for the determination of important aroma compounds in black currant (Ribes nigrum L.) juice, using nasal impact frequency profiling. Journal of Agricultural and Food Chemistry, v. 52, p.1647-1652, 2004. Disponivel em: <>. Acesso em 15 out. 2012. Doi 10.1021/jf035133t.

WANG, Y. et al. Recent advances in headspace gas chromatography. Journal of Liquid Chromatography and Related Technologies, v.31, p.1823-1851, 2008. Disponivel em: <>. Acesso em 22 nov. 2012. Doi 10.1080/10826070802129092.

WERKHOFF, P. et al. Vacuum headspace method in aroma research: Flavor chemistry of yellow passion fruits. Journal of Agricultural and Food Chemistry, v.46, p.1076-1093, 1998. Disponivel em: <>. Acesso em 22 nov. 2012. Doi 10.1021/jf970655s.

Gilberto Costa Braga (I) Adna Prado (II) Jair Sebastiao da Silva Pinto (II) Severino Matias de Alencar (II)

(I) Centro de Ciencias Agrarias, Universidade Estadual do Oeste do Parana (Unioeste), Rua Pernambuco, 1777, 85960-000, Marechal Candido Rondon, PR, Brasil. E-mail: Corresponding author.

(II) Laboratorio de Bioquimica e Analise Instrumental, Departamento de Agroindustria, Alimentos e Nutricao (LAN), Escola Superior de Agricultura "Luiz de Queiroz" (ESALQ), Universidade de Sao Paulo (USP), Piracicaba, SP, Brasil.

Recebido 03.06.13 Aprovado 21.04.14 Devolvido pelo autor 13.10.14 CR-2013-0777.R2

Table 1--Volatile profile of yellow passion fruit juice
(P. edulis f Flavicarpa Deg.) tentatively identified
by GC/MS (DB5 column) and extracted by the static-headspace
(S-HS) (30 compounds) and headspace solid-phase
microextraction (HS-SPME)(44 compounds).


        S-HS   HS-SPME   Volatile compound

1       602    603       Ethyl acetate
2       778    782       Ethyl butanoate
3       790    -         Butyl acetate
4       981    982       Butyl butanoate
5       985    987       Ethyl hexanoate
6       993    995       (3z)-3-Hexenyl acetate
7       997    -         Ethyl 2-hexanoate
8       1001   1002      Hexyl acetate
9       1092   1092      Propyl hexanoate
10      1104   1104      Hexyl propanoate
11      -      1167      Benzyl acetate
12      1190   1191      (3z)-3-Hexenyl butanoate
13      1193   1194      Ethyl (4z)-4-octenoate
14      1196   1198      Hexyl butanoate
15      1202   1202      Ethyl octanoate
16      -      1206      Ethyl 3-octenoate
17      1217   1217      Octyl acetate
18      1242   1242      Hexyl 2-methylbutanoate
19      -      1295      Hexyl pentanoate
20      -      1380      1-Pentyl-2-propenyl butanoate
21      1384   1386      (3z)-3-Hexenyl hexanoate
22      1389   1392      Hexyl hexanoate
23      -      1394      4-Oxocyclohexyl acetate
24      -      1398      Ethyl decanoate
25      -      1463      Ethyl cinnamate
26      1554   1554      Hexyl octanoate
27      974    975       [beta]-Pinene
28      1010   1011      [rho]-Cimene
29      1014   1016      Limonene
30      1027   1028      (Z)-[beta]-Ocimene
31      1038   1040      (E)-[beta]-Ocimene
32      1049   1050      [gamma]-Terpinene
33      1082   1083      [alpha]-Terpinolene
34      1114   1115      (E)-4.8-Dimethyl-1. 3.7-nonatriene
35      843    845       Hexanol
36      1066   1066      Octanol
37      1096   1097      Linalool
38      -      1180      4-Terpineol
39      -      1261      (Z)-3.7-Dimethyl-2.6-octadien-1-ol
40      -      1279      Decan-1-ol
41      -      1102      Nonanal
42      -      1210      Decanal
43      -      1226      [beta]-Cyclocitral
44      -      1451      Geranylacetone
45      -      1482      [beta]-Ionone
46      -      601       Acetic acid
Total   30     44

        --* Relative area %--

        S-HS                  HS-SPME

1       0.16 [+ or -] 0.05    0.03 [+ or -] 0.01
2       16.86 [+ or -] 0.32   3.42 [+ or -] 0.63
3       0.31 [+ or -] 0.03    -
4       0.15 [+ or -] 0.01    0.07 [+ or -] 0.05
5       21.15 [+ or -] 0.29   11.11 [+ or -] 1.08
6       5.16 [+ or -] 0.10    6.23 [+ or -] 0.12
7       0.11 [+ or -] 0.01    -
8       7.96 [+ or -] 0.06    6.51 [+ or -] 0.63
9       0.06 [+ or -] 0.02    0.17 [+ or -] 0.03
10      0.07 [+ or -] 0.01    0.13 [+ or -] 0.02
11      -                     0.18 [+ or -] 0.02
12      1.62 [+ or -] 0.03    3.26 [+ or -] 0.05
13      0.64 [+ or -] 0.03    1.71 [+ or -] 0.16
14      9.75 [+ or -] 0.10    11.88 [+ or -] 0.14
15      0.64 [+ or -] 0.02    1.40 [+ or -] 0.03
16      -                     0.09 [+ or -] 0.01
17      0.08 [+ or -] 0.00    0.28 [+ or -] 0.02
18      0.07 [+ or -] 0.00    0.29 [+ or -] 0.02
19      -                     0.32 [+ or -] 0.03
20      -                     0.12 [+ or -] 0.00
21      1.74 [+ or -] 0.19    6.48 [+ or -] 0.34
22      9.49 [+ or -] 0.74    17.47 [+ or -] 1.33
23      -                     0.66 [+ or -] 0.05
24      -                     0.12 [+ or -] 0.01
25      -                     0.26 [+ or -] 0.04
26      0.07 [+ or -] 0.01    0.45 [+ or -] 0.03
        79.09 [+ or -] 2.02   72.64 [+ or -] 4.85
27      4.15 [+ or -] 0.32    2.32 [+ or -] 0.07
28      0.10 [+ or -] 0.01    0.06 [+ or -] 0.01
29      2.21 [+ or -] 0.16    1.19 [+ or -] 0.01
30      0.40 [+ or -] 0.04    0.23 [+ or -] 0.02
31      9.48 [+ or -] 0.39    5.85 [+ or -] 0.07
32      0.25 [+ or -] 0.03    0.21 [+ or -] 0.01
33      1.55 [+ or -] 0.11    1.46 [+ or -] 0.08
34      1.43 [+ or -] 0.13    0.62 [+ or -] 0.04
        19.57 [+ or -] 1.19   11.94 [+ or -] 0.31
35      0.77 [+ or -] 0.05    2.16 [+ or -] 0.82
36      0.10 [+ or -] 0.01    1.81 [+ or -] 0.15
37      0.63 [+ or -] 0.03    1.89 [+ or -] 0.18
38      -                     0.64 [+ or -] 0.03
39      -                     0.31 [+ or -] 0.04
40      -                     0.12 [+ or -] 0.03
        1.50 [+ or -] 0.09    6.93 [+ or -] 1.25
41      -                     0.32 [+ or -] 0.06
42      -                     0.29 [+ or -] 0.07
43      -                     0.08 [+ or -] 0.01
44      -                     0.23 [+ or -] 0.04
45      -                     0.10 [+ or -] 0.01
46      -                     0.62 [+ or -] 0.97
Total   96.85 [+ or -] 1.59   93.58 [+ or -] 1.25

        Identification (a)

1       MS, KI (b), KI (c)
2       MS, KI (b), KI (c)
3       MS, KI (d)
4       MS, KI (b),
5       MS, KI (b)
6       MS, KI (b)
7       MS,
8       MS, KI (b), KI (d)
9       MS, KI (b), KI (f)
10      MS, KI (b),
11      MS, KI (b), KI (f)
12      MS, KI (b), KI (c), KI (f)
13      MS, KI (b),
14      MS, KI (b), KI (c), KI (f)
15      MS, KI (b), KI (f)
16      MS, KI (b),
17      MS, KI (b), KI (g),
18      MS, KI (b), KI (c),
19      MS, KI (b), KI (c),
20      MS
21      MS, KI (b), KI (c), KI (f)
22      MS, KI (b), KI (c), KI (f)
23      MS
24      MS, KI (b), KI (f)
25      MS, KI (b), KI (f)
26      MS, KI (f)
27      MS, KI (b), KI (c)
28      MS, KI (b), KIe
29      MS, KI (b), KI (f)
30      MS, KI (b), KI (c), KIe,
31      MS, KI (c), KI (f),
32      MS, KI (b),
33      MS, KI (b), KI (c),
34      MS,
35      MS, KI (b), KI (c)
36      MS, KI (b), KI (c), KI (f)
37      MS, KI (b), KI (d), KI (d)
38      MS, KI (b), KI (g), KI (f)
39      MS, KI (b), KI (f)
40      MS, KI (b), KI (f)
41      MS, KI (b), KI (c), KI (g), KI (f)
42      MS, KI (b), KI (g), KI (f)
43      MS, KI (b), KI (c),
44      MS, KI (b), KI (c), KI (f)
45      MS, KI (b), KIe, KI (f)
46      MS, KI (b), KI (c)

* mean [+ or -] standard deviation (n=3)

(a) MS, Comparison of mass spectra from Wiley8 library
and NISTdatabase (

(a) KI, comparisons with the linear retention indices
(Kovats Index) from the literature.

2010; KI (d) DU et al., 2011; KI (e) MAHATTANATAWEE et al., 2007;

KI (f);
KI (g) BYLAITE & MEYER, 2006.
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Title Annotation:texto en ingles
Author:Braga, Gilberto Costa; Prado, Adna; Pinto, Jair Sebastiao da Silva; de Alencar, Severino Matias
Publication:Ciencia Rural
Date:Feb 1, 2015
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