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Plant Foods Hum Nutr (2009) 64:62–67 DOI 10.



Effect of the Temperature on the Spray Drying of Roselle Extracts (Hibiscus sabdariffa L.)
Salvador Gonzalez-Palomares & Mirna Estarrón-Espinosa & Juan Florencio Gómez-Leyva & Isaac Andrade-González

Published online: 10 December 2008 # Springer Science + Business Media, LLC 2008

Abstract The effect of the drying temperature on the volatile components and sensory acceptance of the Roselle (Hibiscus sabdariffa) extract in powder was investigated. The Roselle extraction was carried out by maceration with 7 L of 30% ethanol (v/v), 560 g of fresh Roselle calyces for 168 h. The Roselle extracts were spray dried at different temperatures 150, 160, 170, 180, 190, 200 and 210 °C, giving different outlet values about yield and final moisture. The volatile compounds in Roselle extract and dried samples were performed using needles of solid phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS HP-5890). Twenty volatile compounds were identified in the extracts among them terpenoids, esters, hydrocarbons and aldehydes. Fourteen volatile compounds were identified in the powder sample, but only ten were present in the Roselle extract. This indicates that some compounds were lost and some others were generated due to a degradation process. An acceptS. Gonzalez-Palomares : J. F. Gómez-Leyva : I. Andrade-González (*) Graduate and Research Studies Department, Instituto Tecnológico de Tlajomulco, Km. 10 Carr. San Miguel Cuyutlán, CP 45640 Tlajomulco de Zúñiga, Jal., México e-mail: S. Gonzalez-Palomares e-mail: J. F. Gómez-Leyva e-mail: M. Estarrón-Espinosa Centro de Investigación y Asistencia en Tecnología y Diseño del Estado de Jalisco, A.C. Av., Normalistas No. 800. Colinas de la Normal, CP 44270 Guadalajara, Jal., México e-mail:

ability sensory analysis showed that the best powder sample was the Roselle extract dehydrated using temperature between 190 °C and 200 °C (p <0.05). There was not statistically significant difference in the pH of Roselle extracts ranging from 3.4 to 3.9. It was concluded that the spray drying temperature of the Roselle extracts has an effect on the volatile compounds losses. Keywords Roselle powder . Sensory analysis . Spray dryer . Volatile components

Introduction Roselle calyx (Hibiscus sabdariffa) is the plant part of greatest interest because the calyx is utilized in the processing of fruit preserves, jellies and jams for its rich content in pectin, ascorbic acid and anthocyanin color [1– 3]. Today, the Roselle calyces are utilized as a good source of natural food colorants by their high natural pigment content [4–6]. In addition, Hibiscus sabdariffa anthocyanins have been reported to possess antioxidative, antitumor and anticarcinogenic activity [7–9]. Nevertheless, Hibiscus sabdariffa anthocyanins are unstable during the heat treatments, therefore studies on drying process conditions are requested in order to achieve the best stability of the final product [10]. The obtaining of Roselle powder through spray drying is an important alternative method for the use of the calyces [11–13]. The dehydrated products then can be added easily to other foods to improve their storage, transportation and shelf-life. This classifies the spray drying method as the best alternative to obtain colorants and natural powder flavoring [14–16]. Many studies on Roselle (Hibiscus sabdariffa) powder have been focused on the factors that are influencing the reconstitution characteristics

33 μm film thickness) a capillary column.4. The characteristics of the roselle extracts were 22% of soluble solids and pH of 3. After. The roselle extracts were kept under refrigeration at 4 °C. and physicochemical characteristics of the powder produced [12]. For this reason. Twenty milliliters of Roselle extract were placed in a 40 mL amber headspace vial. 200 and 210 °C. A flexible plastic tube was inserted inside one container and connected to a variable flow peristaltic pump. A HewlettPackard 5890 Series II gas chromatograph with flame ionization detector (FID) coupled to 5972 MSD quadrupole mass spectrometer was used. The HP5890 chromatograph was equipped with HP-1 (50 m×0. A Büchi rotavapor was used to concentrate the samples and to separate all the ethanol at 40 °C. The objective of this work was to evaluate the effect of the spray drying temperatures on the Roselle extracts (Hibiscus sabdariffa L. The reconstituted samples were stored in amber-colored glass flasks and refrigerated until their analysis. Six grams of each sample were placed in an aluminum dish and introduced in a vacuum stove with a temperature of 40 °C until the weight remained constant. only scare studies have been reported on this issue for volatiles in Roselle [6]. changes on the spray drying temperature can affect the concentration of volatile compounds which would generate the loss of some sensorial characteristics [17–20]. An ATAGO refractometer was used to determine the percentage of soluble solids. The outlet temperature was fixed in 80 °C and the atomization was kept at 37. Volatile Analysis of Roselle Extracts by SPME-GC-MS The extraction of volatile compounds from the matrix of the Roselle extracts was carried out by solid-phase microextraction (SPME). A fiber coated with 50/30 mm of divinylbenzene/carboxen on polydimethylsiloxane (DVB/ Carboxen/PDMS. for the spray drying process in all the experiments. Spray Drying A NIRO spray dryer (with the capacity to evaporate 40 kg of water per hour) with a wheel rotating atomizer was used . Mexico during October and November 2006. the quantitative and qualitative analysis by gas chromatography and mass spectrometry (GC-MS) as well as sensorial assays are useful tools in the evaluation of the effect of certain process variables about the quality of the dehydrated products [23–26]. Seven different spray drying temperatures were used. 22]. the retention of the volatile compounds and the sensorial acceptance of the reconstituted spray dried samples. A magnetic stirrer was used for mixture homogenization. 170. The fresh calyces were washed for quick dipping over water distilled. 160.2 mm ID×0. the macerated extracts were filtered through a 150 μm mesh. 180. The Roselle powder samples obtained by spray drying were weighed and packed in their respective amber-coloured glass flasks of 100 mL. the extraction of volatile substances by micro extraction in a solid phase (SPME). The standardization of the mixture was carried out in all the samples until reaching the same concentration of soluble solids of the liquid extract (22%) [12]. These were stored in containers with silica for future analysis. 150.). Operating conditions for GC/ MS were: the oven temperature was programmed at 40 °C Materials and Methods Roselle Extracts Samples Fresh Roselle calyces (with 79% humidity) were collected from an experimental field in Michoacan.06 [27]. Reconstitution of Roselle Powder The reconstituted samples were carried out by placing a portion of Roselle powder in 300 mL of distilled water. An ORION potentiometer was used to measure the pH. 190. The vial was fitted with a PTFE-faced silicone septum and put in a thermostatted bath. Determination of Moisture in the Spray Dried Samples of Roselle In the samples of spray dried Roselle the percentage of moisture was measured by the method of the vacuum stove according to the AOAC-934. PA) exposed for 30 min at 60 °C in the headspace of the vial was then immediately inserted into the injection port of the gas chromatograph for 5 min at 240 °C [28]. Bellefonte. After the calyces were crushed manually and deposited in a closed container with 7 L of 30% methanol (v/v). To diminish some degradation effects of compounds and lost of volatile products is very common to use encapsulation agents [21. all under constant conditions of static maceration.Plant Foods Hum Nutr (2009) 64:62–67 63 or the effects of some additives and processes on characteristics of agglomeration and granulation. Although the spray drying is a fast process. In spite of the knowledge that the volatile compounds show low stability at the spray drying temperatures. Supelco. The flexible outlet tube from the pump was directly connected to the liquid fed inlet of the atomizer. in addition of anthocyanin concentrates and the processing conditions.788×g. The content was left in maceration for 168 h with an occasional shaking to increase the extraction capacity at room temperature.

the variety of the Roselle is different. The weight. 20 volatile compounds were identified. Volatile Compounds of the Roselle Powder The Roselle powder was rehydrated to the same soluble solid concentration than the liquid extract to determine the volatile compounds. The control was the original extract.8 mL/min. In this paired preference test. Quantitation was based in area percent corresponding to the identified components in the Total Ion Chromatogram (TIC).64 Plant Foods Hum Nutr (2009) 64:62–67 for 5 min then ramped at 5 °C/min to 240 °C.1 3. 4. The adherence of powder to walls of the drying chamber is a commonly recognized effect in spray drying of solutions containing sugars and solids easy to agglomerate [30]. aldehydes and phenolic derivatives.0 3. Results & Discussion Spray Drying of Roselle Extracts The processing conditions for all the spray drying experiments were kept at the outlet temperature (80 °C) and the atomizer rate (26. helium with a flow rate of 0. All the reconstituted samples were evaluated for sensorial acceptability by pairing a preference test.48 T2 160 74 4. In general. moisture percentage and pH of the Roselle powder dried at different temperatures Treatment Spray drying temperature (°C) Weight (g) Humidity (%) pH T1 150 73 5. The reconstituted samples were chilled at 5 °C for 24 h prior to sensory evaluation. This has two significant reasons: first. Volatile Compounds Identified in the Roselle Extract by SPME and GC-MS In the Roselle extract. These panelists were randomly selected based on availability. analysis of significant minimum difference (DMS) was made. among the Roselle powders to determine differences based on the pick area of each volatile component. which were randomly coded.05). These compounds were limonene. All the samples were run at least in triplicates. who were students and staff members of the Technological Institute of the West Mexico. In all experiments. 12]. Statistical Analysis An Analysis of Variance (ANOVA) using the Statistical Analysis System Software (SAS) and Duncan test at (p >0. there were terpene components. moisture and pH of seven Roselle powder samples obtained by spray drying at different temperature are shown in Table 1.0 3. This is probably due to the nature of the soluble solids. However. This test was used as a measurement of relative preference of one Roselle drink over another. Sensorial Analysis All the powder samples were reconstituted at 12% of soluble solids and slightly sweetened with sugar. Roselle powder showed a noticeable tendency to stick to internal stainless steel surfaces of the drying chamber especially at higher inlet temperature because this temperature increase the feed flow rate [12].44 T5 190 80 3.000 rpm). This implies that the degradation problem in the samples of powder Roselle extracts were not gendered by the SPME analysis method. Jalisco Campus. 29].48 T3 170 74 4. panelists were asked to make a forced choice between the drinks [2.44 T6 200 75 3. Also. was performed with the data obtained from GCMS. only the terpene compounds were similar to another works [6]. linalool and alphaTerpineol. The second is that the isolation method of volatile compounds used in this work did not require boiling temperatures. The paired preference data were analyzed by binomial distribution [23]. interest and regular consumption of Roselle drinks. It is observed that the pH of the powder does not change with different temperature treatment.48 . this indicates that each variety can have different compositions. the name of current Roselle variety and the cited one should be mentioned [1.0 3. In these samples 14 volatile com- Table 1 Weight (grams).0 3. only required an appropriate material of the fiber (DVB/Carboxen/PDMS) and a temperature of 60 °C. injector port and detector temperatures were 220 and 260 °C.0 3. esters. and a glass of water for rinsing and crackers for consumption between samples were supplied.48 T7 210 74 3.0 3. Each panelist was served with 10 mL of chilled reconstituted samples and control in 30 mL clear plastic containers. Volatile compounds were identified by comparison of their retention indices tentatively only by mass spectra library Wiley 275L. The peak areas identified by GC-MS were used as variables. Each panelist received the reconstituted sample in a random order.44 T4 180 78 4. The panel participating in the acceptance evaluation included 50 volunteers (50% females 18–45 years).

The cis-linalool oxide and the furanic linalool oxide Z and E were the product of the chemical degradation of the fatty acids. as shown in Table 2.10 b b a b 1.13 c 0.06 b Volatile compounds generated by chemical degradation Sugar derivatives Furfural 0.35 b 0.69 a 4.76 b Furanic linalool oxide Z and E 0.16 a 0.10 a Linalool 0.06 b 1.50 ab Different letters mean statistically significant difference using Duncan (p <0.10 c 0.70 a Ethyl linoleate 0. Ten of the 14 compounds identified are the same as the ones identified in the liquid extract.20 4. as shown in Table 2.18 a 0.44 a 0. the Roselle extract dehydrated at 190 °C presented the biggest concentration of volatile compounds and the least concentrations of degraded compounds that the other samples obtained from different spray drying temperatures.05 ab ab a b 0.09 c 0.72 a 0.13 a 1.50 0.17 a 0.09 c Fatty acid derivatives cis-Linalool oxide 0. it is important to acknowledge that significant differences exist among the compounds identified in the liquid extract as the compounds identified in the Roselle powder.30 a 1. cislinalool oxide.55 a 0.60 0.80 0.70 ab Alpha-Terpinolene 0. The Duncan’s test was based on the percentage area of the volatile compounds.07 0.12 1. The compounds generated by chemical degradation of the samples during the spray drying were the furfural.14 1.25 ab b a ab 0. Only the compounds the alphaterpinolene. This also was reported in drying Roselle calyces [6].47 b 0. and the eugenol.07 b 1. ethyl hexadecanoate.13 c 0.05 c 0.45 b 0.40 a 0.05 0.18 a 0.20 c T160 160 °C T170 170 °C T180 180 °C T190 190 °C T200 200 °C T210 210 °C 0. and decanal compounds were present in all experiments without significant difference.10 c 0.07 c Decanal 0.71 ab 0.18 a Divers 4-Ethylguaiacol 0.07 b 1.07 ab 0.87 b 0.16 a 0.40 ab 0.29 b 2. This result proved the hypothesis that the drying temperature had an effect on the retention of volatiles compounds.02 c 2.68 a 0. This Table 2 Volatiles identified in the Roselle powder Spray drying temperature (°C) Area (%) T150 150 °C Volatile compounds retained in the powder Terpenoids p-Cymene 0.19 b 0.00 ab 0.15 b 1.80 b 0. Multiple range tests with base in their retention . In addition.70 a 0.10 ab Limonene 1.28 a 0.50 b 0.09 0.00 0.00 ab 0.Plant Foods Hum Nutr (2009) 64:62–67 65 pounds were identified.53 b Ethyl linoleolate 0. furanic linalool oxide Z and E. although there was a decrease in their concentration.16 a 0. cis-linalool oxide.09 ab ab a b 0.10 c 0. derived of the degradation of sugar and fatty acids that were present in the liquid Roselle extract [6].31 b 0.06 0.69 c 0.35 b 3.00 0.06 b 1.05) determined that exist significant difference among the seven treatments realized to obtain Roselle powder at different spray drying temperatures. It was observed that the concentration of the furfural increased because the drying temperature propitiated its formation by degradation of sugars.67 a 0. In Table 2 the compounds of the Roselle powder are shown and the chromatograms are illustrated in Fig.83 a 0.30 d Phenolic derivatives Eugenol 0.08 0. Duncan’s test (p <0.51 ab 4.11 c 0.07 0.28 a 0.04 0.33 a a a a 0.87 a 0.51 c 0. In Fig.05). The eugenol is a compound resulting from degradation of the phenolic compounds as a consequence of the spray drying temperature of the Roselle samples. 1.40 b 4. furanic linalool oxide Z and E and eugenol compounds due to the obtained the changes by the spray drying temperature. Four different compounds were also generated.06 ab ab a b 0.35 a 1.10 c Aldehydes Benzaldehyde 0.68 a 0.85 b 0. 2 is shown the upward behavior of the furfural.10 b Esters Ethyl hexadecanoate 1. According to the analysis of the least significant difference (LSD) carried out among the Roselle powder samples.55 a 0.12 1.13 1.20 b 1.69 a 0.10 0.

T160=40%. T180= 52%. since it contained the highest concentration of ten volatile com- Area (%) 3 2.5 preference: T150=16%. it is clear than there is significant difference on acceptance among the Roselle powders and the original liquid extract according to the preference tests.5 4 3. 2 Effect of spray drying temperature on the concentration of degradation compounds present in Roselle powder Fig. T0 is Roselle liquid original extract . In comparison to the other treatments (different temperatures). where the highest acceptability was for the liquid extract followed by the T190 sample with statistically significant differences (p <0. The major components detected by chromatographic analysis played an important role.5 0 150 160 170 180 190 200 210 70 60 50 40 30 20 10 0 T0 T150 T160 T170 T180 T190 T200 T210 Spray Drying Inlet Temperature (˚C) Furfural Furanic linalool oxide Z and E Cis-linalool oxide Eugenol Treatments at different temperatures (ºC) Fig.5 2 1. this had the lowest percentage of 5 4. Sensorial Analysis According to the sensorial analysis. T170=52%. and T210=12%.5 100 90 80 Acceptance (%) 1 0. 3 Results of the paired preference tests of the Roselle reconstituted powder. Therefore. although the liquid extract has 92% of preference in the same conditions (T0). Figure 3 shows the percentage over the flavor preference among all the samples analyzed.05). T200=12%. Conclusions The inlet air temperature of 190 °C used in the spray the drying of Roselle extract resulted in the best powder in terms of composition regarding the other treatments. 1 Chromatogram of volatile constituents in Roselle powder dried at 190 °C. more than 76% of the panelists showed that preference for the sample T190 than corresponded to 190 °C drying outlet temperature.66 Fig. The time is in minutes Plant Foods Hum Nutr (2009) 64:62–67 indicates that it is difficult to obtain a powder exactly similar to the liquid extract of Roselle.

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