Effects of Drying Process on the Physicochemical Properties of Nopal Cladodes at Different Maturity Stages Margarita Contreras-Padilla, Elsa Gutiérrez-Cortez, María del Carmen Valderrama-Bravo, Isela Rojas-Molina, Diego Germán Espinosa-Arbeláez, et al. Plant Foods for Human Nutrition ISSN 0921-9668 Plant Foods Hum Nutr DOI 10.1007/s11130-011-0265-x 1 23 Your article is protected by copyright and all rights are held exclusively by Springer Science+Business Media, LLC. This e-offprint is for personal use only and shall not be selfarchived in electronic repositories. If you wish to self-archive your work, please use the accepted author’s version for posting to your own website or your institution’s repository. You may further deposit the accepted author’s version on a funder’s repository at a funder’s request, provided it is not made publicly available until 12 months after publication. 1 23 Author's personal copy Plant Foods Hum Nutr DOI 10.1007/s11130-011-0265-x ORIGINAL PAPER Effects of Drying Process on the Physicochemical Properties of Nopal Cladodes at Different Maturity Stages Margarita Contreras-Padilla & Elsa Gutiérrez-Cortez & María del Carmen Valderrama-Bravo & Isela Rojas-Molina & Diego Germán Espinosa-Arbeláez & Raúl Suárez-Vargas & Mario Enrique Rodríguez-García # Springer Science+Business Media, LLC 2011 Abstract Chemical proximate analysis was done in order to determine the changes of nutritional characteristics of nopal powders from three different maturity stages 50, 100, and 150 days and obtained by three different drying processes: freeze dried, forced air oven, and tunnel. Results indicate that nopal powder obtained by the process of freeze dried retains higher contents of protein, soluble fiber, and fat than the other two processes. Also, freeze dried process had less effect on color hue variable. No changes were observed in insoluble fiber content, chroma and lightness with the three different drying processes. Furthermore, the soluble fibers decreased M. Contreras-Padilla (*) : M. d. C. Valderrama-Bravo División de Investigación y Posgrado, Facultad de Ingeniería, Universidad Autónoma de Querétaro, Cerro de las campanas s/n, C.P. 76010 Querétaro, Qro, México e-mail: [email protected] E. Gutiérrez-Cortez : M. d. C. Valderrama-Bravo : R. Suárez-Vargas Laboratorio Experimental Multidisciplinario LEM-A. Ingeniería en Alimentos, Departamento de Ingeniería y Tecnología, Facultad de Estudios Superiores Cuautitlán, Universidad Nacional Autónoma de México, Av. 1 de mayo s/n, Cuautitlán Izcalli C.P.54740 Edo. de México, México I. Rojas-Molina Facultad de Ciencias Naturales, Licenciatura en Nutrición Universidad Autónoma de Querétaro, Av. de las Ciencias s/n, C.P. 76230 Querétaro, Qro, México D. G. Espinosa-Arbeláez : M. E. Rodríguez-García Departamento de Nanotecnología, Centro de Física Aplicada y Tecnología Avanzada, Universidad Nacional Autónoma de México, Campus Juriquilla No. 3001, Juriquilla, C.P. 76230 Querétaro, Qro, A.P.1-1010, México with the age of nopal while insoluble fibers and ash content shows an opposite trend. In addition, the luminosity and hue values did not show differences among the maturity stages studied. The high content of dietary fibers of nopal pad powder could to be an interesting source of these important components for human diets and also could be used in food, cosmetics and pharmaceutical industry. Keywords Drying . Nopal cladodes . Nutritional characteristics . Opuntia ficus-indica . Physicochemical properties Introduction The Opuntia ficus-indica is a family of plants that are drought tolerant and can be cultivated in arid and semiarid regions. Nopal pads (or cladodes) have played an important role in the Mexican people’s diet and have been used since prehispanic times. Young cladodes are eaten as a vegetable mainly in Mexico and in South of USA. Saenz [1] reported that a potential source of dietary fiber can be found in the nopal due to its high levels of total fiber. It was found that the nopal has a higher concentration of calcium and dietary fiber in more maturity stages than young cladodes [2, 3]. The β-carotene and lutein levels were higher in nopal pads than in other vegetables [4, 5]. Contreras-Padilla et al. [6] found a low concentration of calcium oxalate in nopal cladodes for all maturity stages studied. Scientific studies have reported positive medical effects of nopal, such as: diuretic, antinflammatory, analgesic, antiulcerous, antihyperglycemic, and hypercholesterolemic [7–9]. Applications in the food industry have found that the inclusion of 4% of nopal powder improves rheological properties and increases the calcium content at level of traditional nixtamalized corn Author's personal copy Plant Foods Hum Nutr flour [10]. However, nopal pads are prone to rapid microbiological decay, because of their high water content and low pH, consequently limiting fresh marketing. It is important to keep in mind that older nopal cladodes are not consumed and thus, do not have commercial value which represents an economical loss for farmers. Therefore, postharvest technology is crucial to maintain their quality and in to maximize storage life for human consumption. Drying and grinding processes produce powder forms of material that have several important advantages, such as: it is easy to store and to transport because it is lightweight, and this also extends the shelf-life of the product. Some studies were done regarding the kinetics of drying of nopal [11–14] and others on the impact of drying processes on textural properties [13] and antioxidant components [15, 16]. However, it is necessary to conduct further studies on the effect on the nutritional components and physicochemical parameters due to the drying process in order to obtain products with appropriate nutritional quality for human consumption. The objective of this research was to investigate the effects of three different drying processes: forced air oven drying, freeze-drying, and tunnel drying on the physicochemical and nutritional attributes of nopal pads in three different maturity stages. initial environmental conditions during the drying process were 39% HR and 30 °C. The cladodes were cut into squares of 2×2 cm for the forced air and tunnel process and thickness used was 0.44, 0.65 and 1.045 cm for the different maturity stages, 50, 100 and 150 days, respectively. All the samples were cut to half their original thickness. A forced air oven has a fan and a series of resistors that permits the heated air to move through the trays. Tunnel dryers heat the air which travels through the sections containing product. Force Air Drying The cladodes pieces were placed on stainless steel trays in order to be dried in a force air oven (BG model E102 USA). The drying heat conditions were 50 °C with air flow rate of 1.4 m/s. The amount of nopal pads used was 5 kg and the total drying time was 12 h. Freeze Dried The nopal pads were blended in order to obtain a puree mixture which was frozen in an ultra freezer for 24 h at −50 °C. Then the samples were freeze dried using a freeze zone Labconco equipment with 130×10−3 mbars vacuum and a temperature of −46 °C for 4 days. The amount of nopal used for each sample was 1 kg. Materials and Methods Tunnel Drying Sample Preparation Nopal pads of Opuntia ficus-indica var. redonda, from the experimental field located in Silao, Gto., Mexico, were cultivated during a period of six months and were harvested during May–June 2010. The variety redonda, at present, is cultivated in Guanajuato by a group of producers for human consumption in diverse forms, such as powder, strip, dehydrated cube, spicy, salty, and frozen nopal. Also, some producers are interested in exporting this material. In order to discern the age of cladodes, these were marked and dated during the sprouting, and harvested in three different ages: 50, 100, 150 days. Each sample consisted of 50 kg of nopal pads which were collected from several plants in the same sampling areas but at different maturity stages. All the samples were harvested between 11 am and 12 pm. Once collected, the cladodes were washed with distilled water and disinfected using commercial 10% sodium hypochlorite solution in order to eliminate microorganisms. Then the spines were manually removed. Nopal pieces were placed on stainless steel trays and put into the drying tunnel (Didacta Italia, IC106D). The drying heat conditions were 70 °C and air flow rate of 2.14 m/s. The drying time was 9 h. The amount of each sample was 0.5 kg. The dried pieces were ground using a Pulvex 200 (Mexico) equipment. The grinding feed rate was 10 g/s. The screen output restriction of mill was 0.8 mm. Chemical Proximate Analysis of the Nopal Powder and pH Determination Moisture content was determined using the 934.01 method, nitrogen content using the Kjeldahl method (2001.11), fat content by 920.39 method, ash content by 942.05 method, finally soluble and insoluble dietary fibers were determined according to the 991.42 and 993.19 AOAC Official Methods [17]. Also, the pH values of the nopal powders were determined according to method 44–19 from AACC [18] using a Oakton pH 1,100 series. Drying and Grinding Process Color Analysis of the Nopal Powder The initial average moisture of the cladodes was 92.2% for 50 days, 91.9% for 100 days, and 91.8% for 150 days. The The system used to measure the color was CIELAB. The GretagMacbeth color eye 7,000 spectrophotometer was Author's personal copy Plant Foods Hum Nutr Table 1 Dimensions and weight of nopal pads at 50, 100 and 150 days of maturity Maturity (days) 50 100 150 Average % CV Average % CV Average % CV used with the IQC color program. The results were reported as hue (hº), chroma (C*) and lightness (L*) values. Differential Scanning Calorimetric (DSC) Analysis The soluble and insoluble fiber were analyzed, with 94 and 95% purity of lyophilized nopal, respectively, obtained according to the AOAC and used as references. DSC analysis was carried out in a Q100 TA Instruments calorimeter. The samples were placed in aluminum hermetic sealed pans, and were stabilized at room temperature for 15 min, then heated in a ramp at 10 °C/min. Enthalpy and temperature calibrations were performed using pure indium (99.99%). Weight (g) Length (cm) Width (cm) Thickness (cm) 202.355±1.393 0.69 405.785±4.335 1.068 602.305±1.009 0.17 19.22±0.217 1.13 22.12±0.453 2.07 28.22±0.425 1.51 10.556±0.221 2.1 13.228±0.623 4.71 16.72±0.248 1.49 0.88±0.013 1.47 1.292±0.126 9.814 2.09±0.165 7.9 air drying, tunnel drying and freeze dried, and the maturity stage of cladodes which were 50, 100, and 150 days. The Tukey test for mean comparison was used (P<0.05). The Statgraphics XV ® software was used. Results and Discussion Table 1 shows the weight, length, width, and thickness of 20 nopal pads at 50, 100, and 150 days of maturity with a Statistical Analysis All analytical experiments were conducted in triplicate. The experiments were carried out using bifactorial analysis (3×3) where the two factors were: drying process which were forced Fig. 1 DSC thermogram for soluble and insoluble fiber of nopal pads Fig. 2 Effects of drying process and maturity on protein (a), ash (b), and moisture (c) content of nopal powder. Different letter indicate statistical differences (p<0.05). Average moisture content of samples analyzed (in parenthesis in g/100g d.m.) for freeze dried, 50 d (4.3), 100 d (4.22), 150 d (4.25); for forced air oven 50 d (5.55), 100 d (5.38), 150 d (5.41) and for tunnel 50 d (5.95), 100 d (5.73), 150 d (5.58) Author's personal copy Plant Foods Hum Nutr coefficient of variation less than 10%, which represents nopal pads with homogeneous physical characteristics. Figure 1 shows the thermograms of insoluble and soluble fiber. These thermograms provide information related to the endothermic or exothermic processes that results from the heat treatment. According to this figure, the range of temperatures between 50 to 70 °C have no changes in the chemical composition of fiber; which means that this range can be used for the forced air oven and for the tunnel drying. For insoluble fiber, the endothermic peaks located at 100 °C (A) correspond to loss of water in lignin [19] and the peaks located at 284 °C (C) and 340 °C (D) are associated with hemicellulose and cellulose degradation. These results agree to those found by Tsujiyama and Miyamori [20]. Moreover, two endothermic peaks were found for soluble fiber, a transition located at 122 °C (E) associated with mucilage [21] and the transition found at 215 °C (F) is related to the cross linking process of carbohydrates. The kinetic drying obtained for these processes follow the same behaviors of results reported for other authors [11, 12, 14]. The protein content showed a significant statistical difference between treatments (Fig. 2a) for both maturity stages and types of drying processes used (P<0.05). In all the stages of maturity, the protein content was greater for freeze dried samples. The minor concentration of protein can be explained as follows: 1) some reactions between Fig. 3 Effects of drying process and age on insoluble fiber (a), soluble fiber (b), fat content (c), and pH value (d) of nopal powder. Different letter indicate statistical differences (p<0.05). Average moisture content of samples analyzed (in parenthesis in g/100g d.m.) for freeze dried, 50 d (4.3), 100 d (4.22), 150 d (4.25); for forced air oven 50 d (5.55), 100 d (5.38), 150 d (5.41) and for tunnel 50 d (5.95), 100 d (5.76), 150 d (5.58) carbohydrates and proteins occur during drying process that produces volatile compounds [22, 23] and 2) the moisture content of the lyophilized samples was lower than the other dehydrated samples obtained by the forced air and tunnel; therefore, this condition triggers and apparent major concentration of protein in lyophilized samples. The ash content for all the samples studied, in all maturity stages, demonstrated a statistical difference for the drying processes (P<0.05). The difference was found for freeze dried process (Fig. 2c) because the nopal powder in this process had less moisture (around 4%) than the samples for the other two process which was approximately 5.5%. This result was inherent to the lyophilized process that removes more moisture. The environmental conditions were the same, because the different drying processes for a specific stage of maturity were performed at the same time. Therefore, the differences were found reliable to the drying process. In the case of moisture, the three drying processes had significant differences; therefore, the drying process had an important impact on the final moisture of the samples (Fig. 2c). The insoluble fiber was significantly different but only for maturity factor (P<0.05), and it increases with age (Fig. 3a). Similar results were reported by other authors [2, 3]. For insoluble fiber, no degradation was observed in any of the three different drying processes. These results concur Author's personal copy Plant Foods Hum Nutr with the DSC analysis of insoluble fiber. The soluble dietary fibers were significantly different for both, maturity and drying process (Fig. 3b). The content of soluble fiber decreases with age. These results agree with other authors [2, 3]. The different content of soluble fiber observed from the result of the different drying processes was due to the degradation of this fiber during the dehydration process. The freeze dried samples had a higher content of soluble fiber for all maturity stages; therefore, this process had less effect on this compound. León-Martinez et al. [24] found a glass transition temperature of the mucilage at 45 °C. Their results explain the degradation observed on the soluble fiber during the drying processes of tunnel and forced air oven. Mucilage is part of the soluble fiber (around 93%) [25]. The importance of the dietary fiber lies in the fact that it has interesting physiological and beneficial effects in the human body [1, 9, 26]. In addition dietary fibers can be used in order to modify textures and to improve the stability of the food during production and storage [27]. Results indicate that the fat content decreased with age and that the drying processes had a great influence on the final content (P<0.05) (Fig. 3c). The freeze dried samples had the greatest fat content in comparison with the other dried samples. This is because some fat components produce volatile compounds due to the heat treatment during drying [28]; also apparently there is major concentration of fat in lyophilized samples due to its minor moisture content. The content of fat is very low, which this is an advantage if the powders are considered as low fat products. The nopal powders show a low pH, similar results were found by Ayadi et al. [29], this is due to the fact that these kinds of plants have crassulacean acid metabolism that produces acids as part of the metabolic cycle [30] such as malic acid, citric acid, and oxalic acids [8]. The data only indicate statistical differences for drying process (Fig. 3d). Freeze dried samples had significantly different values of pH. A possible explanation is the concentration effect because moisture was smaller. L* shows a high level, 75; therefore, the samples are light (Fig. 4a). Also, none of the factors have a statistically significant effect on Lightness (P<0.05). Consequently, this attribute was not influenced by the drying process or maturity stage. C* values indicate that samples are pale (Fig. 4b). The results indicate that for those of 150 days of age were paler than the other age groups, except for freeze dried samples. This can be explained by considering that cladodes at this maturity stage could more sensitive to heat treatment and had a slight deterioration of chlorophylls. h° showed values of approximately 90°–98° which is a green– yellow tonality (Fig. 4c). The h° data shows that freeze dried samples were greener than the samples using the other dryers. These results indicate that the forced air oven and tunnel affect the color of the nopal powder giving a yellow Fig. 4 Effects of drying process and maturity on color values of hue (a), chroma (b) and luminosity (c) of nopal powder. Different letter indicate statistical differences (p<0.05). Average moisture content of samples analyzed (in parenthesis in g/100g d.m.) for freeze dried, 50 d (4.3), 100 d (4.22), 150 d (4.25); for forced air oven 50 d (5.55), 100 d (5.38), 150 d (5.41) and for tunnel 50 d (5.95), 100 d (5.76), 150 d (5.58) tonality. Then, freeze dried process had less effect on this variable. The data of the three parameters evaluated show that the color of nopal powder was pale green with high lightness. Similar results were reported [1, 29]. The major components present in the nopal powder are: ash, soluble, and insoluble dietary fibers. These results agree with the finding of Saenz [1], Rodriguez-Garcia et al. [2], Hernandez-Urbiola et al. [3], and Ayadi [29]. Conclusions The samples obtained by different drying process showed different effects regarding the chemical content; color and pH. These values were directly influenced by the process, mainly by the heat treatment. The results are important to consider in order to select the appropriate equipment for the drying process. The samples obtained by freeze dried process were evaluated as the best, because they retained the highest content of the nutrients studied and the color was greener than the other samples. The best maturity stage, which could be used Author's personal copy Plant Foods Hum Nutr for human diet, is cladodes of 100 days of maturity. This is because the content of protein is slight higher, also the soluble and insoluble fiber have an intermediate content that might give the beneficial effect of both fibers. High levels of dietary fibers indicate that nopal powder could be an interesting source for these important components in the human diet. In addition nopal powder could become one of the main ways to consume cladodes in many countries around the world. It could prove to be useful not only in the food industry, but also in the cosmetics and pharmaceutical as raw material for the preparation of products of these industries. Acknowledgements We would like to thank C.P. Luis Lorenz for his invaluable cooperation in his farm (NOPALZIN) and Marlene Meza for the technical English revision of this article. References 1. Saenz HC (1997) Cladodes: A source of dietary fiber. 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