Optimization of maltodextrin and carrageenan gum concentration added in spray drying process of pouzolzia zeylanica extract by response surface methodology

Nong Lam University, Ho Chi Minh City 77 Optimization of maltodextrin and carrageenan gum concentration added in spray drying process of Pouzolzia zeylanica extract by response surface methodology Tan, D. Nguyen1∗, & Thuy, M. Nguyen2 1Department of Food Technology, An Giang University, An Giang, Vietnam 2Department of Food Technology, Can Tho University, Can Tho, Vietnam ARTICLE INFO Research paper Received: January 02, 2018 Revised: April 20, 2018 Accepted: May 24, 2018 Keywords Carrageenan Maltodextrin Pouzolzia zeylanica Response Surface Methodology Spray drying ∗Corresponding author Nguyen Duy Tan Email: ndtan@agu.edu.vn ABSTRACT Pouzolzia zeylanica is a kind of medicinal plant which is generally cultivated in Mekong Delta region. It owns many bioactive compounds that are known to possess antioxidant, antimicrobial and anticar- cinogenic properties. This study aimed to optimize additional carrier concentration for spray drying of Pouzolzia zeylanica extract. Response Surface Methodology (RSM) with central composite design (CCD) was applied for optimization and investigation of the influence of maltodextrin (5ö15%, w/v) and carrageenan gum (0.06ö1.0%, w/v) concentration on the physicochemical characteristics of spray dried powder (bioactive compounds, moisture content as well as particle size distribution). The results showed that the optimum concentrations of maltodextrin and carrageenan gum were 8.8% w/v and 0.082% w/v, respectively. At these optimal conditions, the anthocyanin, flavonoid, polyphenol, tannin, moisture content and particle size of obtained spray dried powder were 5.77 mg cyanidin-3-glycoside equivalents (CE)/100 g; 29.49 mg quercetin equivalents (QE)/g; 28.35mg gallic acid equivalents (GAE)/g; 27.44 mg tannic acid equivalents (TAE)/g, 6.55% and 6.09 µm, respectively. Cited as: Nguyen, T. D., & Nguyen, T. M. (2018). Optimization of maltodextrin and carrageenan gum concentration added in spray drying process of Pouzolzia zeylanica extract by response surface methodology. The Journal of Agriculture and Development 17(3), 77-85. 1. Introduction In recent years, there has been growing in- terest in alternative therapies and the thera- peutic use of natural products and in the last decade much attention has been shifted to search for phytochemicals of native and naturalized plants for pharmaceutical and nutritional pur- poses (Oktay et al., 2003; Wangensteen et al., 2004). Pouzolzia zeylanica was reported that it had no oral acute toxicity at the oral dose of 10 g extract powder/kg (Tran et al., 2010) and can be used to treat cough, pulmonary tu- berculosis, sore throat, enteristis and dysentery (Vo, 2012). Many researches showed that this plant contains flavonoids, tannin, carotenoids, quercetin, vitexin, isovitexin, phylanthin, metyl- sterate, β-sitosterol, oleanolic acid, epicatechin, scopolin, apigenin, alkaloids, steroids, glycosides and saponins (Ghani, 2003; Le, 2007; Fu et al., 2012; Saha & Paul, 2012). Therefore, it will be an important material source for processing func- tional products as beverage, instant tea, etc. Spray drying is one of the most commonly used techniques in transforming a large amount of liquid foods into powder form, due to commer- cially costs and final product quality and stability (Favano et al., 2010). Food powders have many benefits and economic potential over their liquid forms such as volume reduction and packaging easier handling and transportation, stable struc- ture and much longer shelf life (Sarabandi et al., 2014). The physicochemical properties of spray- dried powders depend on the process variables www.jad.hcmuaf.edu.vn The Journal of Agriculture and Development 17(3) 78 Nong Lam University, Ho Chi Minh City such as the characteristic of liquid feed including viscosity, flow rate and the drying air in term of pressure and temperature as well as the type of atomizer (Tee et al., 2012). In order to achieve a successful drying process, high molecular weight of drying agent such as maltodextrin, gum needed to be used for reducing stickiness and wall depo- sition in the dryer chamber. Moreover, the drying carrier agent may improve powder recovery and production yield (Goula & Adamopoulos, 2005; Langrish et al., 2007; Martineli et al., 2007). The objective of this study was to evaluate the impact of maltodextrin and carrageenan gum concentration added to spray drying process of Pouzolzia zeylanica extract on the anthocyanin, flavonoid, polyphenol, tannin, moisture content and particle size distribution of dried powder product. The other variables of spray drying pro- cess were maintained constant. 2. Materials and Methods 2.1. Sample preparation Pouzolzia zeylanica plants were collected in March 2015 from An Giang University. They were harvested after one and a half month cultivation, with 20-30 cm in height. The plants were then washed with tap-water, air-dried until the final moisture content about 12%, cut into small pieces with the length of about 2-3 cm, were extracted with water using airtight extractor. The stirring rate, temperature, time and ratio of solvant and raw material of extraction process were main- tained in 90 rpm, 810C, 30 min and 27:1 v/w, respectively. The hot extract was filtered through cotton cloth and their quantity was determined. The extract was next blended with maltodextrin and carrageenan gum at different concentration following experimental design before spray drying process. The inlet hot air temperature and feed flow speed of spray drying process were 1800C and 18 rpm, respectively. Drying process was car- ried out in a laboratory scale spray dryer (SD-05, LabPlantTM, United Kingdom), with co-current flow regime, the flow rate of drying air was fixed at 60 m3h−1 and the atomizing air was 1.1 bar. 2.2. Powder product analysis Physical characteristics: residual moisture con- tent and total content solids of the product were measured using the infrared humidity analyzer (model AND MS-50, Japan). The particle size of the different samples were obtained in the parti- cle analyzer (model ZEOL-5500, Japan). Bioactive compounds: the anthocyanin con- tent was determined by using the pH differen- tial method (Ahmed et al., 2005; Santos et al., 2013). The results were expressed as mg cyanidin- 3-glycoside equivalents (CE) per gram product. The aluminum chloride colorimetric method was used for flavonoids determination and the amount of flavonoid was calculated as quercetin equiv- alent (QE) per gram of product (Eswari et al., 2013; Mandal et al., 2013). The polyphenol con- tent was determined by Folin-Ciocalteu reagent method and the results were expressed as mil- ligrams of gallic acid equivalents (GAE) per gram of product (Hossain et al., 2013). Tannin content was determined by Folin-Denis method and the results were showed as milligrams of tannic acid equivalents (TAE) per gram of product (Laiton- jam et al., 2013). 2.3. Experimental design and data analysis In order to evaluate the effect of maltodex- trin (5 to 15%, w/v) and carrageenan gum (0.06 to 0.10%, w/v) concentration on moisture con- tent, particle size distribution and bioactive com- pounds (anthocyanin, flavonoid, polyphenol and tannin content), a full factorial design (32) was applied with five replicates in the center point of the experiment design to fit the surface plot for the responses and to estimate the pure er- ror of the multiple regression models, totaling 13 sample preparations (Table 1). The experimen- tal design and statistical analysis were performed using Statgraphics Plus version 15.0 (SYSTAT Software Inc., Richmond, CA, USA) (Myers et al., 2009). A quadratic equation (second degree polynomial equation) was used to fit the results: Y = β0 + k∑ i=1 βiXi + k∑ i=1 βiiX 2 i + k−1∑ i=1 k∑ j=2 βijXiXj (i < j) Where Y is the predicted response parame- ter, β0 is a constant, βi, βii and βij are the re- gression coefficients. Xi and Xj are the levels of the independent variables (maltodextrin and car- rageenan gum concentration). Experimental data The Journal of Agriculture and Development 17(3) www.jad.hcmuaf.edu.vn Nong Lam University, Ho Chi Minh City 79 were then fitted to the selected regression model to get a clear understanding of the correlation between each factor and different responses. This was obtained by estimating the numerical val- ues of the model term (regression coefficients), whose significance was statistically judged in ac- cordance with t-statistic at confidence interval of 95%. Non-significant (P > 0.05) term was deleted from the initial equation and data were refitted to the selected model. The quality of the math- ematical models fitted by RSM was evaluated by ANOVA, based on the F-test, the probability value (Pvalue) of lack-of-fit and on the percentage of total explained variance (R2) and also on the adjusted determination coefficient (R2adj), which provide a measurement of how much of the vari- ability in the observed response values could be explained by the experimental factors and their linear and quadratic interactions (Table 2). A simultaneous optimization using the desirability function was performed in order to maximize the anthocyanin, flavonoid, polyphenol, tannin con- tent and to minimize moisture content and par- ticle size distribution. 3. Results and Discussion 3.1. Effect of matodextin and carragennan concentration on bioactive compounds In spray drying processing, bioactive com- pounds can be often destroyed by thermal air. Thus, the supply of maltodextrin and car- rageenan gum into Pouzolzia zeylanica extract to reduce bioactive compounds damage and im- prove physicochemical characteristics of obtained powder by gel particle formation mechanisms of polysaccharide to protect bioactive compounds during spray drying process (Burey et al., 2008) (Figure 1). Figure 1. Schematic of gel particle formation mech- anisms. The result showed that anthocyanin, flavonoid, polyphenol and tannin content changed from 2.42 to 5.85 mg CE/100g; 20.63 to 29.30 mg QE/g; 27.39 to 28.35 mg GAE/g and 25.83 to 27.43 mg TAE/g powder product (Table 1), respectively. The bioactive compounds were presented in final products which depended on the supplemental carrier percent of maltodextrin and carrageenan. The concentration of carrageenan gum and maltodextrin had a positive quadratic effect (P < 0.01) on anthocyanin content. The anthocyanin content increased with increasing carrageenan gum concentration in approximately 0.075 to 0.095% (w/v) and achieved optimal values at 0.083%. Besides, anthocyanin content was also achieved high values in maltodextrin concentra- tion approximately 7 to 10% (w/v) and reached an optimum of 8.88% (Figure 2a). It could be noticed in Figure 2b that levels of carrageenan gum had slight quadratic influence (P < 0.05) to flavonoid content in product. The flavonoid content achieved high values with carrageenan gum concentration of range from 0.065 to 0.10% (w/v) and reached optimum values in the car- rageenan gum concentration of 0.082%. Whereas the concentration of maltodextrin had a clear quadratic impact (P < 0.01) on flavonoid con- tent in product. The flavonoid content achieved high values in maltodextrin concentration from 5 to 9% (w/v) and the optimum values obtained at maltodextrin concentration of 7.38%. The car- rageenan gum concentration had slight quadratic impact (P < 0.05) on the polyphenol content in the product. However, the maltodextrin lev- els had significant quadratic effect on polyphenol content (P < 0.01). The high polyphenol content was obtained when using the carrageenan gum concentration from 0.07 to 0.10% (w/v) and op- timal values was achieved at 0.086%. In addition, the polyphenol content increased with maltodex- trin concentration increases in the range from 5 to 11% (w/v) and the optimum value was found at 6.83% of maltodextrin concentration (Figure 2c). The response surface and contour plot in Figure 2d showed that carrageenan gum concentration had significant quadratic influence (P < 0.01) on tannin content in the product, whereas the mal- todextrin levels had slight quadratic effect on tan- nin content. A high tannin content was obtained when us- ing carrageenan gum concentration from 0.07 to 0.095% (w/v) and the highest value was achieved at 0.084% of carrageenan gum. Moreover, the high tannin content was obtained when using the maltodextrin percent ranging from 5 to 15% www.jad.hcmuaf.edu.vn The Journal of Agriculture and Development 17(3) 80 Nong Lam University, Ho Chi Minh City T a b le 1 . C o d e a n d rea l va lu es o f m a lto d ex trin a n d ca rra g en n a n co n cen tra tio n a n d resu lts fro m p h y sico ch em ica l p ro p erties a n a ly sis o f sp ray d ried p ow d er N u m b er ru n F acto rs R esp o n ses va ria b les M alto d ex trin (% , w /v ) C arragen n a n (% , w /v ) A n th o cya n in (m g / 1 0 0 g ) F lavo n o id (m g / g ) P o ly p h en o l (m g / g ) T a n n in (m g/g) M oistu re (% ) P article size (µ m ) 1 1 0 (0 ) 0.08 (0 ) 5 .5 9 2 9 .0 5 2 8 .1 3 2 7 .43 6.45 6.04 2 1 5 (+ 1 ) 0.1 (+ 1 ) 3 .2 9 2 3 .3 8 2 7 .3 9 2 5 .93 7.31 6.51 3 1 5 (+ 1 ) 0.08 (0) 3 .3 8 2 2 .2 5 2 7 .7 5 2 7 .16 6.89 6.44 4 1 0 (0 ) 0.08 (0 ) 5 .7 8 2 8 .1 9 2 8 .2 5 2 7 .39 6.49 6.15 5 1 0 (0 ) 0.08 (0 ) 5 .7 5 2 9 .3 0 2 8 .3 2 2 7 .43 6.52 6.18 6 5 (-1) 0.06 (-1) 3 .9 1 2 8 .2 9 2 7 .7 5 2 5 .83 7.75 6.14 7 1 0 (0 ) 0.08 (0 ) 5 .8 5 2 8 .8 6 2 8 .3 3 2 7 .37 6.47 6.13 8 1 0 (0 ) 0.06 (-1) 4 .2 5 2 7 .5 7 2 7 .9 2 2 6 .63 7.21 6.23 9 5 (-1) 0.1 (+ 1 ) 4 .1 5 2 8 .2 0 2 8 .2 6 2 7 .20 7.61 6.19 1 0 1 0 (0 ) 0.1 (+ 1) 5 .0 7 2 8 .2 9 2 8 .0 8 2 6 .69 6.95 6.24 1 1 5 (-1 ) 0.08 (0 ) 4 .9 4 2 9 .1 8 2 8 .3 2 2 7 .31 7.25 6.09 1 2 1 0 (0 ) 0.08 (0) 5 .6 6 2 9 .1 4 2 8 .3 5 2 7 .24 6.52 6.09 1 3 15 (+ 1) 0.06 (-1) 2 .4 2 2 0 .6 3 2 7 .4 3 2 6 .71 7.68 6 .54 The Journal of Agriculture and Development 17(3) www.jad.hcmuaf.edu.vn Nong Lam University, Ho Chi Minh City 81 T a b le 2 . M a th em a ti ca l eq u a ti o n s th a t d es cr ib e th e re sp o n se va ri a b le s (a n th o cy a n in , fl av o n o id , p o ly p h en o l, ta n n in , m o is tu re co n te n t a n d p a rt ic le si ze ) in re sp o n se to m a lt o d ex tr in a n d ca rr a g ee n a n g u m co n ce n tr a ti o n s R es p on se va ri ab le s R eg re ss io n eq u a ti o n 1 R 2 R 2 (a d ju st ed fo r d .f .) P v a lu e (l a ck -o f- fi t) A n th o cy an in (m g C E /1 00 g) Y = −1 3 .0 01 + 35 9 .4 3 7X 1 + 0 .8 6 2 X 2 − 2 2 4 4. 4 X 2 1 + 1 .5 7 5 X 1 X 2 − 0 .0 5 6 X 2 2 0 .9 8 7 0 .9 7 8 0 .0 7 7 F la vo n oi d (m g Q E /g ) Y = 14 .0 77 + 27 3 .4 4 3X 1 + 1 .1 8 9 X 2 − 1 9 7 6. 7 2 X 2 1 + 1 .1 8 9 X 1 X 2 − 0. 1 2 X 2 2 0 .9 8 9 0 .9 8 2 0 .6 0 3 P ol y p h en ol (m g G A E /g ) Y = 21 .4 73 + 13 9 .3 4 5X 1 + 0 .2 6 4 X 1 − 7 5 2 .1 5 5 X 2 1 − 1. 3 7 5 X 1 X 2 − 0. 0 1 1 X 2 2 0 .9 7 4 0 .9 5 6 0 .9 1 7 T an n in (m g T A E /g ) Y = 9. 43 4 + 37 0 .7 3X 1 + 0 .6 0 6 X 2 − 1 9 3 0. 6 X 2 1 − 5. 7 7 5 X 1 X 2 − 0. 0 0 7 X 2 2 0 .9 9 7 0 .9 9 5 0 .0 6 6 M oi st u re co n te n t (% ) Y = 17 .8 57 − 22 2 .6 67 X 1 − 0 .4 1 4 X 2 + 1 3 8 7 .5 X 2 1 − 0. 5 7 5 X 1 X 2 + 0 .0 2 2 X 2 2 0 .9 9 4 0 .9 8 9 0 .0 8 1 P ar ti cl e si ze (µ m ) Y = 7. 86 9 − 39 .6 55 X 1 − 0. 0 6 7 X 2 + 2 4 7 .8 4 5 X 2 1 + 0 .0 0 5 X 2 2 0 .9 5 4 0 .9 3 9 0 .7 8 5 1 X 1 = C a rr a g e e n a n g u m c o n c e n tr a ti o n (% , w / v ); X 2 = M a lt o d e x tr in c o n c e n tr a ti o n (% , w / v ). www.jad.hcmuaf.edu.vn The Journal of Agriculture and Development 17(3) 82 Nong Lam University, Ho Chi Minh City Figure 2. Response surface and contour plots for anthocyanin (a), flavonoid (b), polyphenol (c) and tannin (d) content in different maltodextrin and car- rageenan gum concentrations. (w/v) and an optimum value was found at mal- todextrin concentration was 8.19%. The content of compounds (anthocyanin, flavonoid, polyphenol and tannin) increased with increasing the maltodextrin concentration from 5 to 9% and this compound content decreased when using maltodextrin from 9 to 15%. The maltodextrin and carrageenan gum con- centrations were significant quadratic impact on bioactive compounds in product. The bioactive compounds achieved the high values when the concentrations of maltodextrin and carrageenan gum were added to the extract in the range from 6.8 to 8.8% and 0.082 to 0.086%, respec- tively. Bhusari & Kumar (2014) also showed the polyphenol content was increased when increas- ing the concentration of added carrier agent. Maasniza et al. (2013) reported that the best quality of Garcinia powder with additional mal- todextrin concentration was 5%. The beetroot- orange juice powder was also obtained with the best functional properties and the conservation of betalain was high when using 5% of maltodex- trin (Ochoa-Martinez et al., 2015). The best qual- ity of Ber powder was obtained with encapsu- lating material, with 8% maltodextrin (Singh et al., 2014), whereas the use of maltodextrin/pectin with 10:1 ratio (11% w/v) led to encapsulate 3% w/v polyphenol-rich extract forming a stable powder made up of well-formed and micronized particles suitable for storage and handling (San- sone et al., 2011). The pink guava powder pro- duced with 15% of maltodextrin was found to be more convenient than other concentrations. The obtained powder had a low moisture content and was more stable with the highest bulk density (Shishir et al., 2015). The obtained pequi pulp powder with high nutritional quality (vitamin C, carotenoid) found at additional maltodextin con- centration was 18% (Santana et al., 2016). 3.2. Effect of maltodextrin and carragennan concentration on moisture content and particle size of powder product The moisture content had an influence on the quality of the powder (Goula et al., 2004). The re- sults in Figure 3a showed that the additional car- riers concentration also had significant quadratic impact on the moisture content of spray dried powder product (P < 0.01). The moisture con- tent was decreased in increasing maltodextrin and carrageenan gum concentration. The low moisture content was obtained when using mal- todextrin and carrageenan gum at concentration varied from 9 to 12% and 0.075 to 0.09%, respec- tively. The lowest moisture content was achieved at maltodextrin of 10.59% and carrageenan gum of 0.082%. The study result was also similar to the result reported of Fernandes et al. (2012), Wang & Zhou (2013), & Sabhadinde (2014). The concentration of maltodextrin used for develop- ment of the Pouzolzia zeylanica powder varied between 5 to 15% (w/v). The maltodextrin con- centration using in this study was less than 10 to 30% that were used by Abadio et al. (2004), Tonon et al. (2008), & Kha et al. (2010). Mois- ture content of sample decreased with increasing maltodextrin concentration from 5 to 9%. Abadio et al. (2004) also found a decrease in moisture content in final pineapple juice powder with an increase of the maltodextrin concentration from 10 to 15% (w/v). A higher concentration of mal- todextrin used could increase the concentration of feed solids and could reduce the content of to- tal moisture for evaporation (Grabowski et al., 2006). Carrageenan gum concentration had no ef- fect on particle size with P < 0.05. The mean par- ticle size was increased with increasing the mal- todextrin concentration (Figure 3b). The result from Sharifi et al. (2015) revealed that concentra- tion of maltodextrin increased from 7.5 to 15%, SEM micrographs of the powder indicated the in- creasing trend in particle size as a result of in- The Journal of Agriculture and Development 17(3) www.jad.hcmuaf.edu.vn Nong Lam University, Ho Chi Minh City 83 Figure 3. Response surface and contour plots for moisture content (a) and particle size (b) in different maltodextrin and carrageenan gum concentrations. crease of concentration of maltodextrin as drying aid. However, Fernandes et al. (2012) reported that no correlation was found between particle size distribution and different carbohydrate con- centration. A statistical analysis was performed on the ex- perimental results to obtain the regression mod- els. ANOVA was used to evaluate the significance of each variable on the model. The quadratic model for all the response in terms of coded fac- tors are shown in Table 2. The goodness-of-fit of the regression model showed that the exper- iment and predicted data were fitted and the coefficient of determination R2 > 0.8 (Guan et al., 2008). In addition, the probability value of lack-of-fit was non-significant (P > 0.05) (Za- beti et al., 2009). The results of ANOVA anal- ysis showed that the linear, quadratic and inter- action factors of maltodextrin and carrageenan gum concentration had effects on anthocyanin, flavonoid, polyphenol, tannin and moisture con- tent of obtained powder product with the reli- ability of 95%. However, the carrageenan levels were not effective on particle size, so regression equation of particle size did not have interac- tion factor of carrageenan gum and maltodex- trin concentration. The coefficient of determina- tion of the predicted models in the response was R2 > 0.954, R2adj > 0.939 and lack of fit had P > 0.05. These values would give a relatively good fit to the mathematic model. Moreover, the correla- tion between experimental and predictable data of goal functions such as anthocyanin, flavonoid, polyphenol, tannin, moisture content and particle size are also shown in Figure 4. 3.3. Multiple response optimization The simultaneous optimization of multiple re- sponses might be a main concern for industrial applications (Tsai et al., 2010). The energy cost of the process significantly diminished when ex- Figure 4. Correlation between the experimen- tally and the estimated values for anthocyanin (a), flavonoid (b), polyphenol (c), tannin (d), moisture content (e) and particle size (f) using the models de- scribed in equation 2, 3, 4, 5, 6, 7, respectively (as shown in Table 2). traction parameters were optimized (Spigno et al., 2007). The response variables including an- thocyanin, flavonoid, polyphenol, tannin, mois- ture content and particle size were optimized sep- arately; therefore, they allowed the targeting of a certain class of compounds only by varying the spray drying process parameters. Yet, the desir- ability function in the RSM was utilized to reveal the combination of the parameters (maltodextrin and carrageenan gum concentration) which are capable of simultaneously maximizing or mini- mizing the responses. The overplay plot shows the outlines superposition of all the studied re- sponses and the simultaneous optimum for all re- sponses is shown by the black spot (Figure 5) showing the best experimental parameters that maximize bioactive compounds content and min- imize powder product characteristics. The black spot showed the optimum for all the responses. Figure 5. Superposition plots. www.jad.hcmuaf.edu.vn The Journal of Agriculture and Development 17(3) 84 Nong Lam University, Ho Chi Minh City 4. Conclusion The effects of the concentration of maltodex- trin and carrageenan gum on the powder quality of the spray dried Pouzolziazeylanica extract had successfully been investigated by factorial exper- imental design. The result of simultaneous op- timum for all responses showed that the opti- mum supplemental carrier concentrations to pro- duce spray dried powder with the highest con- tent of bioactive compounds, the lowest moisture content and the smallest particle size were ob- tained when the blending of maltodextrin and carrageenan gum concentration was 8.8% and 0.082%, respectively. References Abadio, F. D. B., Domingues, A. M., Borges, S. V., & Oliveira, V. M. (2004). Physical properties of pow- dered pineapple (Ananas comosus) juice effect of mal- todextrin concentration and atomization speed. Jour- nal Food Engineering 64(3), 285-287. Ahmed, J. K., Salih, H. A. M., & Hadi, A. G. (2005). 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