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Production and characterization of camel milk powder enriched with date extract

Jawaher AlYammahi, K. Rambabu, A. Thanigaivelan, Shadi W. Hasan, Hanifa Taher,


Pau Loke Show, Fawzi Banat

PII: S0023-6438(23)00215-3
DOI: https://doi.org/10.1016/j.lwt.2023.114636
Reference: YFSTL 114636

To appear in: LWT - Food Science and Technology

Received Date: 21 November 2022


Revised Date: 23 February 2023
Accepted Date: 4 March 2023

Please cite this article as: AlYammahi, J., Rambabu, K., Thanigaivelan, A., Hasan, S.W., Taher, H.,
Show, P.L., Banat, F., Production and characterization of camel milk powder enriched with date extract,
LWT - Food Science and Technology (2023), doi: https://doi.org/10.1016/j.lwt.2023.114636.

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Author Statement

Jawaher AlYammahi: Conceptualization, Methodology, Software, Investigation, Formal analysis,


Writing – original draft

K Rambabu: Investigation, Data curation, Writing – original.

A Thanigaivelan: Visualization, Data curation.

Shadi W. Hasan: Validation; Writing – review & editing.

Hanifa Taher: Validation; Writing – review & editing.

Pau Loke Show: Investigation, Data curation.

f
Fawzi Banat: Project administration; Writing – review & editing; Funding acquisition, and Supervision.

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1 Production and Characterization of Camel Milk Powder Enriched with Date

2 Extract

3 Jawaher AlYammahia, K Rambabua, A Thanigaivelana, Shadi W. Hasana,b, Hanifa

4 Tahera, Pau Loke Showc, Fawzi Banata,*


a
5 Department of Chemical Engineering, Khalifa University, P.O Box 127788, Abu Dhabi,

6 United Arab Emirates


b
7 Center for Membranes and Advanced Water Technology (CMAT), Department of Chemical

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8 Engineering, Khalifa University of Science and Technology, Abu Dhabi, P.O. Box 127788,

9 United Arab Emirates

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Department of Chemical and Environmental Engineering, Faculty of Science and Engineering,
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11 University of Nottingham Malaysia, Jalan Broga, 43500 Semenyih, Selangor Darul Ehsan,
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12 Malaysia

13 *Corresponding author:
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14 Prof. Fawzi Banat: fawzi.banat@ku.ac.ae


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23 Graphical Abstract

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25
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26 ABSTRACT

27 The production of camel milk powder, rich in date fruit extract, has not been studied yet. In

28 this study, a spray-drying technique was used to produce camel milk powder enriched with

29 date sugar. The optimum operating conditions were determined using response surface

30 methodology to maximize the overall powder yield. A maximum overall yield of 55 wt./wt.%

31 was achieved by operating at a temperature of 160 °C, a flow rate of 7.0 mL/min, a

32 concentration of 3.1 wt./v% MD, and outlet air temperature of 100 ℃ . In addition, the powder

33 was analyzed and characterized physically, chemically, optically and nutritionally. Results

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34 showed relatively good functional properties (high cohesion, low moisture content, good

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35 solubility and color properties) and unique morphological properties (amorphous, roundish

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microparticles with a broader particle size distribution). Further, DSC, TGA, and chemical
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37 analysis results showed that date sugar fortified camel milk powder (DCMP) had improved
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38 thermal stability and high nutritional value. Spray-dried DCMP might find applications in a
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39 wide range of food and beverage products.


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41 Keywords: date sugar; maltodextrin; encapsulation; camel milk powder; optimization; spray

42 drying.

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44 1. Introduction

45 The number of undernourished people in the world reached 768 million in 2020, indicating

46 the severity of the food insecurity problem and the urgent need to find innovative, highly

47 nutritious products from unutilized and under-utilized food resources (FAO, 2020). The use of

48 dietary supplements containing high-value phytochemicals, such as vitamins, minerals, and

49 others, has shown a remarkable reduction in the cases of certain diseases related to malnutrition

50 (Pocobelli et al., 2009). Recently, fruit and milk-based beverages have received considerable

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51 attention worldwide as a source of protein, vitamins, minerals, and other phytochemicals. In

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52 the food industry, the nutritional value of protein-rich food is mainly determined by

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bioavailability, composition (such as amino acid profile and total protein content), and

54 processing conditions. Among the many protein-rich dairy products available worldwide,
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55 camel milk has witnessed considerable attention lately due to its nutritional value and medicinal
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56 properties. It is made up of several bioactive compounds, such as essential amino acids,


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57 vitamins, lactose, minerals, and functional proteins with anti-diabetic, antibacterial, and anti-
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58 cancer properties (Khatoon & Najam, 2017). Furthermore, bioactives such as lactoferrin,
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59 peptides, zinc, and monounsaturated and polyunsaturated fatty acids present in camel milk help

60 combat or reduce the risk of various diseases, such as gastrointestinal diseases, tuberculosis,

61 autism, jaundice, and asthma (Swelum et al., 2021). Interestingly, camel milk was found to be

62 a safer and healthier option for lactose-intolerant patients (Ho et al., 2022). Moreover, camel

63 milk is homologous to human milk due to its unique composition. Therefore, it is considered a

64 good alternative to human milk for infants (Sabahelkhier et al., 2012). Despite the great

65 nutritional value and health benefits of camel milk, its consumption is still very limited

66 compared to bovine milk. This could be due to the salty flavor that makes it unappealing to

67 humans, especially children. The findings from the literature study analyzing the consumer

68 acceptance, preferences and attitudes to camel milk suggests the need for further research to
69 improve the sensory quality of camel milk and the possible application of flavors as an option

70 to cover the perceived salty taste of camel milk (Profeta et al., 2022). To overcome this

71 problem, camel milk could be enriched with natural high-value fruit extract as a flavoring

72 agent.

73 Date fruit is an excellent natural healthy flavoring source due to its sweet taste and concentrated

74 nutritional components (Siddiqi et al., 2020). Date fruit contains a high amount of sugar,

75 ranging from 60 to 70% by weight, which is easily assimilated by human metabolism

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76 (Samarawira et al., 1983). Many dates in the United Arab Emirates (UAE) contain a substantial

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77 amount of reducing sugars (fructose and glucose) (Rambabu et al., 2020). The nutritional

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analysis of eleven date fruit varieties commonly cultivated in the UAE was extensively studied,

79 and the results indicated that all varieties contained a reasonably significant amount of
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80 micronutrients (K, Mg, Ca, and P), glutamine, protein, and aspartic amino acids, along with
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81 other essential amino acids (Rambabu et al., 2020). Furthermore, date fruits contain a good
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82 amount of dietary fiber, ranging from 6.5 to 11.5%, of which 6-16% are soluble, and 84-94%
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83 are insoluble. Accordingly, dates consumption can help to meet the balanced diet requirements,
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84 having 14-g fiber for every 1000 calories of food consumed each day (Alasalvar & Shahidi,

85 2013; Ghnimi et al., 2017; Sidhu, 2006). Studies have shown that dates have low glycemic

86 indices, and their consumption by patients with diabetes did not result in significant

87 postprandial glucose excursions (Alkaabi et al., 2011). The UAE is one of the world’s leading

88 producers of date fruits and fresh camel milk. In 2020, the UAE produced 58,176 tons of fresh

89 camel milk and 328,669 tons of date fruits (FAO, 2020). Thus, the combination of camel milk

90 and date fruits would be an exceptionally nutritious superfood that can help prevent

91 malnutrition, especially in the Arab world, due to their availability and known nutritional and

92 therapeutic values. Recent studies have reported the nutritional benefits of adding date fruit to

93 camel milk (Aljutaily et al., 2021; Ho et al., 2022; Tawfek et al., 2021).
94 To manage the surplus of fresh milk produced daily and enable the worldwide distribution of

95 high-quality milk-based products, drying processes are considered to increase their shelf life

96 and ease the transportation process. Spray-drying is an important processing technology used

97 in many food and nutraceutical applications (Murugesan & Orsat, 2012). This drying technique

98 is preferable for foods containing heat-sensitive components due to the short drying time and

99 low temperature of the end product. It is more advantageous than other drying methods due to

100 easy installation, short residence time, lower cost, and the ability to maintain the chemical and

101 biological stability of the product (A. Verma & Singh, 2015). The spray-drying technique,

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102 known to quickly remove moisture from atomized liquid droplets, results in a continuous fast

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103 process, more economical operation, and flexibility in handling various feeds (Zouari, Schuck,

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et al., 2020). The surface morphology of the camel milk powder produced using the freeze-
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105 drying technique was described as a porous sheet-like structure, while the camel milk powder
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106 produced using the spray-drying technique was agglomerates of individual near-spherical
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107 particles (Deshwal et al., 2020). The product or powder’s yield and quality depend on the

108 efficiency of the system (inlet temperature, the outlet temperature, relative humidity, and the
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109 flow rate of the drying gas, as well as the aspirator speed ) and the powder collection
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110 capabilities (A. Verma & Singh, 2015).

111 Stickiness is one of the major problems that restrict the spray-drying process of sugar-rich food

112 products due to the high hygroscopicity of low-molecular-weight saccharides, such as fructose

113 and glucose, which actively assimilate molecules of water and are suspended in ambient

114 humidity (Schenz et al., 1985). Therefore, while spray-drying sugar-rich materials, there are

115 certain operational problems and increased losses due to product stickiness to the wall of the

116 dryer chamber or powder agglomeration in the collection container (A. Verma & Singh, 2015).

117 Factors that contribute to the stickiness problem are the higher hygroscopicity of the amorphous

118 powder, the increase in the solubility of sugars with temperature, and the lower melting point
119 and the glass transition temperature (Tg) (Bhandari et al., 1997). Other problems, such as

120 viscous flow and caking or clumping, start to develop upon exposure to water and after the

121 storing and packaging process of the product (Schenz et al., 1985). Drying aids, carrier agents,

122 or antiplasticizer agents, such as maltodextrin with different dextrose equivalents (DE), gum

123 arabic, starch, and isolated protein, are added to reduce stickiness and agglomeration problems

124 by increasing Tg, thus obtaining free-flow powder with improved product stability (Sablani et

125 al., 2008). Several published studies have compared different carrier materials based on the

126 resulting product yield. Maltodextrin (77%) was found to be more effective than gum arabic

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127 (68%) as a carrier material for the drying of sour cherry and it was used as carrier for red wine

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128 lees polyphenolics encapsulation (Can Karaca et al., 2016; Ricci et al., 2022). In the last decade,

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many attempts have been made to optimize the processing conditions to produce high-quality
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130 camel milk powder for longer shelf life (Deshwal et al., 2020; Habtegebriel et al., 2021;
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131 Habtegebriel, Edward, et al., 2018; Habtegebriel, Wawire, et al., 2018; Ho et al., 2019; Perusko
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132 et al., 2021). The unique functional components in milk, such as whey protein and lactose,

133 which act as wall materials for many micronutrients during drying processes, allow the creation
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134 of microencapsulates and crusts with increased encapsulation efficiency (Aadinath et al.,
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135 2017). Milk and dairy milk enrichment with bioactives such as vitamins, essential fatty acids,

136 phenolic compounds, minerals, and enzymes through several encapsulation techniques such as

137 spray-drying, freeze drying, extrusion gelation, coacervation, emulsification, and liposomal

138 encapsulation has been reviewed by Adinepour, Pouramin, Rashidinejad and Jafarial (2022)

139 (Adinepour et al., 2022).

140 To the best of our knowledge, no study has been conducted on the production of camel milk

141 powder enriched with date fruit extract. Therefore, in this study, the production of camel milk

142 powder enriched with date sugar was investigated using a spray-drying technique as an

143 encapsulation technique. Design of experiments was performed using Central Composite
144 Design, and the results were subjected to an optimization study to determine the operating

145 conditions for maximum overall powder yield. The spray-dried date fortified camel milk

146 powder obtained under optimal conditions was physically analyzed by determining the bulk

147 density, color, moisture content, and solubility of the sample, chemically by FT-IR and

148 nutritional analysis, morphologically by optical and electrical microscopy techniques, and

149 thermally by TGA and DSC.

150

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151 2. Materials and methods

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152 2.1 Chemicals and reagents

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The date fruit powder was purchased from a local market in Al Ain, UAE, and stored at 4 °C
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154 before the experiments. According to the manufacturer, the Sukkari date fruit powder was
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155 produced by sun-drying and grinding processes. Camel milk powder (CMP) was used instead

156 of fresh liquid camel milk to avoid the evaporation process prior the spray-drying and to
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157 accurately calculate the overall yield based on the feed content. The used CMP was obtained
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158 from a leading local market in the UAE. Maltodextrin (MD) with the dextrose equivalent of
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159 10-17 was purchased from Sigma-Aldrich Co. (Germany). Deionized (DI) water (conductivity

160 0.05 µS/cm) was used for the sample preparation throughout the work.

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162 2.2 Feed preparation for spray-drying

163 Date fruit powder (DP) was dissolved in deionized water at a liquid to solid ratio of 7.6 mL/g.

164 The mixture was placed inside the ultrasound bath (USC-THD, VWR, UK) after setting the

165 conditions at 50% sonication power, a temperature of 60 °C, and an extraction time of 30 min.

166 Upon completion of the extraction, the solution system was vacuum filtered to separate the

167 extract from the spent date fruit powder. Subsequently, a concentrated solution of camel milk
168 fortified with date fruit extract (DFE) was prepared by adding 30% (wt./v) of camel milk

169 powder, and a certain amount of MD (% wt./v) was added to 100-mL DFE with total soluble

170 solids (TSS) of 11.5 ± 0.5 %. The TSS values were determined using a digital refractometer

171 (PR-101, Atago Co. Ltd., Japan) at 20 °C, and the results were reported as mean ± standard

172 deviation. The mixture was mixed thoroughly by heating at 45 ± 5 °C and stirring at 350 rpm

173 using a hot plate stirrer (MSH-20D, WiseStir, Finland) to improve the drying process by

174 reducing the viscosity of the feed and the surface-free fat in the whole milk powder (Banat et

175 al., 2002). Subsequently, the mixture was directly fed to the spray dryer while it was stirred at

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176 45 °C.

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2.3 Production camel milk powder enriched with date extract by spray-drying
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178 Spray-drying experiments were conducted using a laboratory-scale spray dryer (Büchi mini B-
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179 290, Büchi Labortechnik AG, Switzerland) equipped with a dehumidifier (B-296, Switzerland)

180 and a two-fluid nozzle with a standard diameter of 0.7 mm. The spray dryer has a co-current
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181 airflow configuration, which is commonly used in the food industry and is suitable for heat-
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182 sensitive materials. Initially, hot air was blown through the drying chamber for 10–15 min to
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183 stabilize the inlet air temperature, then the feed was introduced into the spray dryer through a

184 peristaltic pump. The aspirator (%) was fixed at 100% (37.5 m3/h) to enhance the drying

185 capacity and overall yield. The air flowmeter was set at 40 mm height to allow uniform

186 spraying. Other parameters were varied to optimize the process conditions for maximum

187 powder yield. Once the feed was fully processed, the air was cooled to room temperature, after

188 which the powder was collected from the drying cylinder, the cyclone separator, and the

189 collection vessel. The powder was collected and kept in plastic bags. The DCMP powder

190 samples were then stored in a desiccator until the analysis stage. The overall powder yield was

191 calculated as the ratio of spray dry powder weight to the weight of processed solid matter in

192 the feed (Tontul & Topuz, 2017):


𝑀𝑝𝑜𝑤𝑑𝑒𝑟 (𝑔) (1)
𝑌0 (wt./wt. %) = × 100%
𝑀𝑃𝑆𝑀 (𝑔)

𝑀𝑃𝑆𝑀 (𝑔) = (𝑀𝑇𝑆𝑆 ) + 𝑀𝐶𝐴 + 𝑀𝐶𝑀𝑃 (2)

193 Where 𝑀𝑝𝑜𝑤𝑑𝑒𝑟 is the weight of the powder collected from the collection vessel and cylinder,

194 𝑀𝑃𝑆𝑀 is the weight of the processed solid matter, 𝑀𝑇𝑆𝑆 is the TSS present on the date sugar

195 extract, 𝑀𝐶𝐴 is the carrier agent (MD) weight, and 𝑀𝐶𝑀𝑃 is the camel milk powder weight.

196 [Figure 1]

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197 2.4 Experimental design

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198 2.4.1 Optimization (RSM-FCCD) -p
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199 The Response Surface Methodology (RSM) with complete random Central Composite Design
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200 (CCD)-Face cubic points (FCC) was used to optimize the spray-drying process conditions with

201 the objective of maximizing the overall yield. CCD with three factors and three levels (-1, 0,
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202 and +1) was used to generate 20 runs, including six repeats at the center point. The independent
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203 variables were air inlet temperature (120, 140, and 160°C), feed flow rate (2, 6, and 10
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204 mL/min), and MD concentration (1.15, 2.88, and 4.60 wt./v%). The matrix of the experimental

205 design with the coded and un-coded levels is given in Table 1. The overall yield 𝑌𝑜 (wt./wt.%)

206 was taken as responses for this optimization study and outlet air temperatures 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 (°C) was

207 recorded due to its importance. Analysis of variance (ANOVA) (with a 95% confidence

208 interval) was carried out to evaluate the effect of the independent variables, namely air inlet

209 temperature (X1), feed flow rate (X2), and MD concentration (X3). Regression analysis was

210 performed to fit the experimental data using a second-order empirical polynomial model and

211 to establish the relationship between the independent variables and the responses. The

212 statistical model was used to determine the optimal conditions for the maximum extraction

213 yield, which was then experimentally validated. The used mathematical model equation is:
3 3 3 (3)
2
Y = b0 ∑ bn Xn + ∑ bnn Xn + bnm ∑ bnm Xn Xm
n=1 n=1 n≠m=1

214 where Y is the response, b0 is the model constant, and bn, bnn, bnm are the model coefficients.

215 X represents the factors studied with linear terms (Xn), and their two-way interaction terms

216 (XnXm), and quadratic terms Xn2.

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218 2.4.2 Statistical analysis

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219 Minitab software v 19.1 (Minitab Inc, Pennsylvania, USA) was used to perform the statistical

220 analysis, and the ANOVA test, p-values <0.05 were considered statistically significant. All

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analyses were performed in duplicates, and their values were expressed as mean ± standard
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222 deviation (SD).
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223
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224 2.5 Physical and functional analysis


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225 The physical parameters of the spray-dried DCMP obtained under optimal conditions, such as
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226 moisture content, bulk density, flowability, solubility, and color, were determined. The

227 moisture content was measured by drying 3 g of DCMP at 70 ºC to constant weight (Rafiee

228 Darsangi et al., 2020). The bulk density is one of the important properties of powders, as it

229 determines the ease of handling and transportation of the powder. The bulk density of the

230 product was determined by freely pouring 1 g of the powder into a 10 mL graduated cylinder

231 (readable at 0.2 mL) without tapping or disturbances. Afterward, the graduated cylinder was

232 lifted and gently dropped against its weight, the volume was recorded again, and the tapped

233 bulk density was calculated. The volume occupied by the sample was recorded, and the loose

234 and tapped bulk densities were calculated (Habtegebriel, Edward, et al., 2018).
𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑜𝑤𝑑𝑒𝑟 (𝑔) (4)
𝐿𝑜𝑜𝑠𝑒 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 (𝑔/𝐿) =
𝐵𝑢𝑙𝑘 𝑝𝑜𝑤𝑑𝑒𝑟 𝑣𝑜𝑙𝑢𝑚𝑒 (𝐿)

𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑜𝑤𝑑𝑒𝑟 (𝑔) (5)


𝑇𝑎𝑝𝑝𝑒𝑑 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 (𝑔/𝐿) =
𝑇𝑎𝑝𝑝𝑒𝑑 𝑝𝑜𝑤𝑑𝑒𝑟 𝑣𝑜𝑙𝑢𝑚𝑒 (𝐿)

235 The flowability and cohesiveness of DCMP were evaluated in terms of Carr’s index (CI) (Carr

236 Jr, 1965) and Hausner ratio (HR) (Hausner, 1967), which were calculated on the basis of loose

237 and tapped bulk densities. The equations used to calculate CI and HR were:

𝑇𝑎𝑝𝑝𝑒𝑑 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 − 𝑙𝑜𝑜𝑠𝑒 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 (6)

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𝐶𝐼 (%) = × 100%

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𝑇𝑎𝑝𝑝𝑒𝑑 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦

𝑇𝑎𝑝𝑝𝑒𝑑 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 (7)

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𝐻𝑅 (%) = × 100%
𝑙𝑜𝑜𝑠𝑒 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 -p
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238 Powder samples with CI values in the range of (0-10) are considered to have an excellent flow,

239 (10–15) good flow, (16-20) fair flow, (21–25) possible flow, and CI values >26 poor flow
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240 characteristics. Furthermore, the powder sample with an HR value >1.2 shows low
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241 cohesiveness, while values in the range (1.2-1.4) and greater than 1.4 are considered
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242 intermediate and high cohesiveness powders, respectively. DCMP solubility was determined
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243 by dissolving 1 g powder in 100 mL of distilled water using a high-speed magnetic stirrer

244 (MSH-20D, WiseStir, Finland). To remove undissolved materials, the mixture was centrifuged

245 at 7500 rpm for 10 min. Then, 25 mL of supernatant was dried at 105 ° C for 5 h, and solubility

246 (%) was measured based on the equation below (Rafiee Darsangi et al., 2020).

𝑚1 − 𝑚2 (8)
𝑆 (%) =
25
𝑚𝑖 ×
100

247 where S is the solubility (%), m1 is the weight of the container after drying (g), m2 is the weight

248 of the empty container (g), and mi is the initial weight (g). The color of the DCMP was

249 determined using a colorimeter (Colorimeter PCE-CSM 5, PCE Instruments, UK) with silicon
250 photoelectric diode sensor, D65 light source, and CIEL*a*b* color space mode. This system

251 employs a* (red-green axis), L* (lightness), and b* (yellow-blue axis) to provide a visually

252 linear color specification. Initially, the colorimeter was calibrated using a white ceramic disk

253 supplied with the unit. To determine the colorimetric parameters, the DCMP was placed in the

254 powder compartment of the powder test box. Parameters such as luminosity (L*), the intensity

255 of red and green (a*), and the intensity of yellow and blue (b*) were measured and recorded.

256 The degree of saturation or chroma (c*) and the hue value (h*) were calculated using the

257 following equations (Vieira et al., 2019).

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𝑐 ∗ = √𝑎∗2 + 𝑏 ∗2 (9)

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𝑏∗
ℎ∗ = 𝑎𝑟𝑐𝑡𝑎𝑛 ( ∗ )
𝑎
-p (10)
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All analyzes were performed in duplicates and their values were expressed as mean ± standard
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259 deviation (SD).


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261 2.6 Morphological and structural analysis

262 The samples (DCMP, CMP, and MD) were placed on thin glass plates and then observed under

263 an optical light microscope (EVOS FLoid microscope, ThermoFisher Scientific, USA)

264 equipped with a fixed 20x objective. For SEM analysis, the DCMP and CMP samples were

265 mounted on aluminum stubs with double-sided carbon adhesive tape and coated with gold-

266 palladium to prevent sample charging. The surface morphologies of the CMP and the spray-

267 dried DCMP were studied with SEM (FEI, Quanta 3D FIB, USA) operated at an accelerating

268 voltage of 20 kV and at different magnification levels (500, 1000, and 5000x). The SEM

269 images were further processed to obtain the diameter using ImageJ software (Schneider et al.,

270 2012). The X-ray diffraction patterns of MD, CMP, and the spray-dried DCMP were measured
271 to investigate the sample’s crystallinity using an X-ray diffractometer (D2 Phaser, BRUKER,

272 USA) at 30 kV and CuKα radiation with a wavelength of 1.54 Å. The powdered samples were

273 carefully placed in the standard sample holder and scanned at diffraction angles between 5°–

274 80° at a scanning rate of 5°/min.

275

276 2.7 Thermal analysis

277 The thermal stabilities of DCMP, CMP, and MD were analyzed using differential scanning

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278 calorimetry (DSC 404, NETZSCH, Germany), calibrated with Indium. DSC measurements of

279 powder samples were carried out under an atmosphere of N2 with a heating scan between 25

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and 250 °C at a heating rate of 10 K/min. Thermogravimetric analysis (TGA) was performed
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281 to evaluate thermal stability by measuring changes in sample weight with the change in
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282 temperature using (STA 449 F3, NETZSCH, Germany). The spray-dried DCMP sample was
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283 heated from 25 ° C to 900 °C at a 10 K/min heating rate under N2 atmosphere. All analyses

284 were performed in duplicates, and their values were averaged.


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286 2.8 Chemical analysis

287 The nutritional analysis of the macro and micronutrients present in the DCMP was carried out

288 through a certified company. Briefly, proximate composition analysis (fat including saturated,

289 monounsaturated and polyunsaturated, total carbohydrates, and proteins) was performed

290 following AOAC standard methods (AOAC 989.05, AOAC 996.01, AOAC 986.25, and

291 AOAC 991.20). Cholesterol content was measured using GC-FID (Beggio et al., 2018).

292 Furthermore, micronutrients such as minerals (sodium, potassium, calcium, and iron) were

293 analyzed using a flame photometer and ICP-AES. Dietary fiber content was determined by

294 enzymatic reaction, followed by distillation and gravimetric analysis. Total sugars and vitamins
295 (A and C) were determined using HPLC techniques. The FT-IR spectra for MD, DFE, CMP,

296 and DCMP were obtained using the FT-IR instrument (ATR FTIR, Bruker ALPHA, UK) in

297 the range of 4000–400 cm−1. Each spectrum was corrected against the background spectrum of

298 air and obtained by taking an average of 32 scans. Spectra were collected and analyzed using

299 the OPUS software (version 4.0, Bruker, France) provided by the equipment manufacturer.

300 Qualitative-elemental analysis of the spray-dried DCMP was performed using FEI model FEG-

301 SEM Quanta 3D FIB equipped with an energy dispersive X-ray analysis (EDS). The analysis

302 was performed at a beam voltage of 20 kV in high vacuum mode. The acquisition time of the

f
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303 spectrums was 300 s. All analyses were performed in duplicates, and their values were

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304 expressed as mean ± standard deviation (SD).
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305
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306 3. Results and discussion

307 3.1 Spray-drying optimization of date-fortified camel milk powder


na

308 RSM-CCD was applied to correlate the effect of the spray-drying operating parameters (feed
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309 flow rate, air inlet temperature, and MD concentration) on the selected response, namely,
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310 overall yield (wt./wt.%). Yield is one of the most important indicators in the food industry,

311 where higher yields mean greater profit. Moreover, the outlet temperature of the drying gas

312 (air) was recorded for all experimental runs due to its significance. It is one of the most

313 important parameters in the spray-drying process, which determines the moisture content of

314 the spray-dried powder. Low outlet air temperature can produce low amount whey protein

315 denaturation and solubility loss (Anandharamakrishnan et al., 2007). Furthermore, a higher

316 temperature difference has been indicated to result in lower energy consumption (Parthasarathi

317 & Anandharamakrishnan, 2017). Therefore, to ensure a low moisture level in the final product,

318 the 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 should be controlled and the difference between the air outlet and the air inlet
319 temperatures (ΔT) should be as small as possible (Habtegebriel, Wawire, et al., 2018). The

320 various experimental operating conditions for the spray-drying of DCMP and the

321 corresponding response values are tabulated in Table 1. It is evident that the overall powder

322 yield ranged between 6.4-57 wt./wt.% and the outlet temperature ranged between 73-107 °C

323 under various operating conditions, indicating the significant effect of all parameters studied

324 on the responses. The maximum overall yield obtained in this study (57 wt./wt.%) is analogous

325 to the maximum yield (61.8 %) obtained when fresh camel milk was spray-dried at 140 °C,

326 5.00 rev/min, and 23 psi (Habtegebriel et al., 2021). In addition, runs no. 15-20, which

f
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327 correspond to the central points of the parameters studied, showed moderate variation in the

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328 responses. This suggests a reasonably good experimental repeatability and viability. In

329
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addition, the relationships between the operating parameters (X1, X2, and X3) of the spray-
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330 drying process and the response values (The overall yield ‘Y1’) were fitted using a second-
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331 order polynomial model, and the regression models obtained are presented below in Eq. (12)
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332 and Eq. (13).


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Y1 = 4.52X1 + 25.46X2 + 11.55X 3 − 0.01142X12 − 0.737X22 − 0.535X32 (11)


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− 0.1180X1 X2 − 0.0308X1 X3 + 0.138X2 X3 − 413

333 Statistical analysis of the quadratic model was performed using ANOVA, and the results are

334 presented in Table 2. It is evident that the experimental data are in a good fit with the fitted

335 models for Y1 at a p-value of 0.001. Additionally, the model's lack of fit was insignificant for

336 the response studied, and tolerability was appropriate. The linear (X1, and X3), square (X2X2),

337 and interaction (X1X2) effects were significant (p < 0.05) in the case of Y1. In addition, the rest

338 of the linear, square, and interaction effects were insignificant (p > 0.05). Fig. S1 shows the

339 Pareto charts for both responses (Y1), which confirm the significant parameters (X1, X3, X2X2,

340 and X1X2) affecting the overall yield (Y1),. Analysis of the data obtained for Y1 indicated that
341 the estimated regression coefficient R2 was 90.33%, Radj2 was 81.6%, and the S value was 6.5.

342 These results suggest that the obtained model fits the experimental data very well. Fig. S2

343 displays residual plots, including the normality plot, histogram, and residual versus fits and

344 order for each model (Y1). The normality plots and histograms obtained from the residuals

345 demonstrate the normal distribution of the data. Residual versus fit and order show the random

346 distribution of the independent residuals, as shown in Fig. S2.

347 The effect of each parameter, namely, the air inlet temperature (120-160 °C), feed flow rate (2-

f
348 10 mL/min), and the MD concentration (1.15-4.60 wt./v%), on the overall yield and the outlet

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349 air temperature (𝑇𝑜𝑢𝑡𝑙𝑒𝑡 ) was evaluated based on the experimental results obtained. Fig. 2 (a

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350 &b) illustrates the effect of air inlet temperature on the overall yield and 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 (ΔT) at a fixed
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351 feed flow of 6 mL/min and MD concentration of 2.88 wt./v %. The increase in the air inlet
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352 temperature from 120 to 160 °C resulted in a progressive increase in the overall yield and
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353 continuous increase in 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 due to the enhanced evaporation rate and the increased heat
na

354 transfer from the drying air to the falling droplet, eventually resulting in efficient drying of the
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355 powder. Similar results were found when the inlet temperature increased (Habtegebriel,
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356 Edward, et al., 2018). The maximum overall yield was obtained at an air inlet temperature of

357 ~ 160 °C. Generally, carrier agents are important for the spray-drying of food-containing fruit

358 juices to overcome stickiness issues that lower the overall efficiency and performance of the

359 process. Therefore, the effect of varying the concentration of the carrier agent (MD) at a fixed

360 feed flow rate (6 mL/min) and air inlet temperature (140 °C) on the overall yield, 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 , and

361 ΔT was analysed (Fig. 2 (e & f). Increasing the MD concentration from 1.15-2.88 wt./v%

362 increased the overall yield and slightly increased the 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 (decrease in ΔT), due to the

363 reduced stickiness (increased glass transition temperature of the feed) and lower

364 hygroscopicity. An additional increase in MD concentrations above 2.88 wt./v% decreased the

365 overall product yield and 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 (increased the ΔT) due to the possible increase in the feed
366 viscosity that negatively impacts the drying performance (Chong & Wong, 2015).

367 Consequently, the optimal MD dose that resulted in the highest overall product yield was above

368 2.88 wt./v%. The variation in the feed flow rate from 2 to 6 mL/min was analyzed at a fixed

369 air inlet temperature of 140 °C and MD concentration of 2.88 wt./v%, and Fig. 2 (e) depicts

370 the significant increase in overall yield due to the sufficient residence time required to

371 evaporate each droplet generated during the spray-drying process. However, an additional

372 increase above 6 mL/min caused a substantial decrease or no further enhancement in overall

373 yield because of the shorter residence time and insufficient drying of the product. Furthermore,

f
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374 at higher flow rates, dripping issues were observed in the dryer chamber due to the un-atomized

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375 feed solution, which was reported in many studies (Banjare et al., 2019; Chegini & Ghobadian,

376
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2007; Tontul & Topuz, 2017). Fig. 2 (f) shows the insignificant effect of the feed flow rate on
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377 the 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 and ΔT (almost constant), where the highest detected temperature was 93 °C at ~6
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378 mL/min. Accordingly, ΔT value was the smallest (46 °C), demonstrating sufficient drying and
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379 a high overall yield. The optimum feed flow rate value that resulted in the maximum overall

380 yield and lowest 𝑇𝑜𝑢𝑡𝑙𝑒𝑡 is 6 mL/min.


ur
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381 The two-way interaction effects were demonstrated using response surface plots (3D surface

382 and contour plots), where each of the fitted models (overall yield) was plotted as a function of

383 two independent variables while maintaining the third variable at the center point (Fig. 3). The

384 interaction effect of the air inlet temperature and the feed flow rate on the overall yield was the

385 most significant (p<0.05). Optimal response results (Y1=54.11%) were predicted using the

386 regression model under the following optimal conditions: 160 °C, 6.93 mL/min, and 3.1% of

387 carrier agent (MD). To validate this predicated optimum (maximum) overall yield value, spray-

388 drying experiments were performed in triplicate at 160°C, 7.0 mL/min, and 3.1 wt./v% MD

389 concentration. The experimental value of Y1 under these optimal conditions was 55.17±0.74

390 wt./wt.%, which is very close to the predicted value.


391 [Figure 2]

392 {Table 1]

393 [Table 2]

394 [Figure 3]

395 [Table 3]

396 3.2 Physical and functional properties of spray-dried powder

f
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397 Functional and reconstitutional properties such as free bulk density, tapped bulk density,

398 flowability, cohesiveness, moisture content, and solubility of commercially available CMP and

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399
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the spray-dried camel milk powder (CMP) fortified with DFE are presented in Table 3. Loose
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400 or free bulk density (FBD) was measured by pouring powder freely into a container, while
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401 packed or tapped bulk density (TBD) demonstrates the performance of the compacted powder.

402 The spray-dried product, DCMP, has an FBD and TBD of 400±10 and 560±20 g/L, while a
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403 pure CMP showed an FBD of 0460±10 g/L and a TBD of 550±20 g/L as shown in Table 4.
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404 The increase in the tapped bulk density of the CMP fortified with date fruit is due to the
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405 incorporation of sugar components into the milk powder and the morphological properties of

406 the spray-dried power (spherical-shaped, smooth surface, smaller particle size, and wider range

407 of particle size distribution) (Habtegebriel, Edward, et al., 2018). Ogolla et al. reported that

408 spray-dried milk powder has FBD and TBD in the range of 390-480 g/L and 400-630 g/L,

409 respectively (Ogolla et al., 2019). Furthermore, the bulk density data were used to estimate the

410 rheological characteristics, such as the flowability and cohesiveness, of spray-dried products.

411 These key parameters are helpful in selecting suitable storage containers or packaging materials

412 for the powder produced. The compressibility and free-flowing characteristics, as well as the

413 cohesiveness of the powder, are presented in terms of Carr’s index (CI) and Hausner ratio (HR),

414 respectively, as shown in Table 4. The results revealed that the CI and HR values were higher
415 for DCMP compared to CMP. Similar results have been reported for spray-dried powder

416 formulated with carrier agents (Adsare & Annapure, 2021; Chandralekha et al., 2017). This

417 could be due to the fact that the encapsulation of date fruit extract and CMP increased the bulk

418 density and, hence, indicated poor flowability and higher cohesiveness for DCMP compared

419 to CMP. The moisture content of the spray-dried product is another important factor that is

420 used to evaluate the performance of spray-drying and determine the water dehydration process

421 in food products. Commercially available CMP and DCMP obtained by spray-drying exhibited

422 a moisture content of 2.40% and 3.67% (w/w), respectively (Table 4). The larger surface area

f
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423 per unit volume sprayed droplet, and the smaller particle size of the powder sample produced

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424 facilitate drying and therefore resulted in a low moisture content that is within the typical final

425
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moisture content range of 2-4% (dry basis) (Amaladhas & Emerald, 2017; Neves et al., 2019).
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426 The low moisture content of the spray-dried product reduces the deteriorative reactions (lipid
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427 oxidation, lactose crystallization, protein denaturation, etc.) and increases the microbiological
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428 stability of the powder obtained, thus making it safe for long-term preservation. Furthermore,

429 the effectiveness and applicability of powder as a food supplement depend on its solubility.
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430 Pure CMP and DCMP showed very close solubility values of about 77%, most probably due
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431 to the small particle size of the powder and the homogeneous mixing of the feed that helped in

432 reducing the surface-free fat and enhancing the powder reconstitution property (Vignolles et

433 al., 2007). The lower solubility of DCMP in water as compared to CMP could be due to the

434 higher fiber content in DCMP (0.81 g/100g) as indicated in the nutritional analysis section

435 below. Martínez et al. observed that higher fiber content decreased water solubility index

436 values in extruded blends of fiber, whey protein concentrate, and corn starch (Martínez-Bustos,

437 F., Viveros-Contreras, R., Galicia-García, T., Nabeshima, E. H., 2011). Solubility can be

438 further enhanced through a multi-stage dryer. Deshwal et al. reported a significantly lower

439 solubility of 65.47% for the spray-dried camel milk powder compared to the freeze-dried
440 sample (88.77%) (Deshwal et al., 2020). However, a higher percent solubility of 96.4% was

441 reported for CMP (Zouari, Mtibaa, et al., 2020). The variation in solubility explicitly depends

442 on the concentration and nature of the carrier agents, drying technology, and operating

443 conditions. For example, Adsare and Annapure reported a decrease in the total solubility of the

444 spray-dried product by increasing the amount of gum Arabic added to curcumin coconut whey

445 (C-CW) (Adsare & Annapure, 2021). Therefore, to obtain the powder with the desired

446 functional properties, a specific formulation regarding the carrier agent and nutritional sugar

447 constituents in the feed solution (milk) should be prepared and processed under optimized

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448 operating conditions. Khulal et al. reported lower solubility of CM protein after fortification

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449 with fruit juices due to increased protein aggregation (Khulal et al., 2021). To enhance the

450
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physical and functional properties of DCMP, multi-stage dryers with the addition of a surface
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451 acrive agent such as lecithin to the feed should be considered to enhance wettability, solubility
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452 and dispersability esspecially for fat-rich powders (Barbosa-Cánovas & Juliano, 2005).
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453 The color attributes of DCMP and CMP were also analyzed using a PCE colorimeter. Sugar-
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454 encapsulated camel milk powder (DCMP) exhibited lower a* (-1.49±0.04), and b* (9.00±0.04)
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455 and higher h* (99.36±0.18) values compared to pure CMP, i.e. a*=8.53±0.15, b* = 27.86±0.01

456 and h* = 72.98±0.28. The color difference is due to the incorporation of sugar constituents

457 (obtained from DFE) into the milk powder. These results are consistent with the colorimetric

458 analysis of coconut whey powder (CWP) encapsulated with the GA (Adsare & Annapure,

459 2021). Figure S3 presents the pictorial image of pure CMP and DCMP obtained from a spray

460 dryer operating under optimal conditions (160 °C, 6.93 mL/min, and 3.1 wt./v % MD carrier

461 agent).

462 [Table 4]

463 3.3 Morphological characterization of spray-dried DCMP powder


464 The drying method and the feed content significantly affect the quality of the DCMP product.

465 Therefore, microscopic images were obtained to analyze the microstructures of the untreated

466 CMP and the spray-dried DCMP with the addition of a carrier agent (MD). The optical

467 microscopic images of pure MD, commercial CMP, and spray-dried DCMP under visible light

468 at a fixed magnification (20x) are shown in Figs. S4 a, b, and c, respectively. It can be observed

469 that the pure MD and CMP showed an irregular shape, whereas the microscopic analysis of the

470 CMP encapsulated with date sugar revealed a micrometric ranged, homogeneous, and regular-

471 shaped powder. Fig S4 (c) displays the multi-wall capsules confirming the successful

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472 encapsultion of DCMP. Detailed analysis of the spray-dried powder morphology and particle

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473 sizes of the commercial CMP and spray-dried product (DCMP) was performed at higher

474
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magnification levels using SEM (FEI, Quanta 3D FIB, USA).
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475 Figs. 4 (a-c) and (d-f) show the SEM images of pure CMP and DCMP, respectively. CMP
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476 exhibited an irregular structure and a smooth surface with a higher degree of agglomerations.
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477 Interestingly, the obtained particles were free of any prominent structural defects, cracks, or
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478 breaks, indicating the preservation of bioactive compounds in the camel milk powder during
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479 spray-drying. Similar SEM images were observed for the spray-dried powder of bovine serum

480 and camel milk, as published in the literature (Deshwal et al., 2020; Kosasih et al., 2016).

481 Comparatively, the spray-dried powder (DCMP) shows multisize spherical microparticles that

482 are much smaller in size that can be easily assimilated or digested than that of the commercial

483 CMP. The size of the particles ranged from 1.2-27.7 µm, with an average diameter size of

484 9.1±7.8 µm. The very small particle size could be attributed to the low initial feed concentration

485 (TSS of 11.5%). The feed’s TSS content of 45-50%, achieved through the pre-concentration

486 (evaporation) process, results in a larger particle size (Amaladhas & Emerald, 2017).

487 Consequently, the higher viscosity of the feed affects the particle size distribution (Roy et al.,

488 2017). The shrinkage of the powder particles (smaller particle size) for the spray-dried DCMP
489 is attributed to the feed properties (low TSS% and viscosity) during the spray-drying process.

490 Similar to the CMP, prominent wrinkles were not observed in the DCMP sample even at a

491 higher magnification of 5000x (Fig. 4 e). Notably, the SEM analysis of DCMP indicates the

492 presence of many small spherical particles with a smooth surface that are attached to the bigger

493 particles that were not observed for CMP. These smaller particles ensure the encapsulation of

494 date sugar and camel milk powder as indicated in other studies of encapsulation through spray-

495 drying (Ruano Uscategui et al., 2018; Santhalakshmy et al., 2015; K. Verma et al., 2022).

496 Therefore, spray-drying could be effectively implemented for the production of nutritious food

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497 supplements by encapsulating date sugar and camel milk. The structural nature of MD, CMP,

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498 and spray-dried DCMP were examined using an X-ray diffractometer, and their respective

499
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diffractograms are shown in Fig. S5. The diffractograms of MD and CMP confirmed the
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500 amorphous nature (see Fig. S5). Similarly, the XRD pattern of the DCMP sample showed an
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501 amorphous state, which is desirable to avoid stickiness and caking issues during the storage of
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502 the DCMP. The amorphous nature of date sugar encapsulated CMP is consistent with the

503 previous studies on curcumin encapsulated milk powder (Liu et al., 2016).
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504 [Figure 4]

505 3.4 Thermal characterization of spray-dried DCMP powder

506 Information about the temperature sensitivity of pure materials (MD, CMP) and spray-dried

507 products (DCMP) is required to understand the influence of temperature on food preservation

508 and formulation. Fig. S6(a) shows the differential scanning calorimetry (DSC) analysis of the

509 carrier agent (pure MD), commercially available CMP, and date sugar fortified CMP (DCMP)

510 obtained through the spray-drying process. Three distinct patterns were observed for the DSC

511 thermograms of MD, CMP, and DCMP. Table S1 displays the peak, onset, and end set

512 temperatures of the materials studied. Pure MD exhibited an endothermic peak at 93.5 °C
513 followed by an exothermic peak indicating its thermal decomposition. CMP sample showed an

514 endothermic peak temperature at 62.1°C. Compared with commercially available CMP (62.1

515 °C), an increase in peak temperature was observed for date-fortified CMP (82.6 °C). The wider

516 peak shape and higher temperature compared to CMP are due to the encapsulation of date

517 sugars (fructose, glucose, and sucrose) and CMP. Similar thermal characteristics were observed

518 for the fruit juice-milk powder produced using the spray-drying technique (Afifi et al., 2009).

519 Furthermore, the DSC results of DCMP confirmed an enhancement in the thermal stability,

520 which is in accordance with the published literature on curcumin powder (Jafari et al., 2016).

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521 Thermogravimetric analysis (TGA) was also performed for the DCMP sample, and the result

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522 is depicted in Fig. S6(b). The thermogram of the spray-dried product (DCMP) exhibited three

523
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distinct thermal evaporation/decomposition zones. The first step in the temperature range of
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524 25-125 °C corresponds to the removal of free and bound water, volatiles, and the fractional
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525 denaturation of proteins in the DCMP. A weight loss of around 2.5-3% was calculated in the
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526 first zone, and the results are in good agreement with the proximate analysis, i.e., the moisture

527 content of DCMP (see Table 4). This indicate that the spray-drying process at air inlet
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528 temperature of 160 °C produced a dry DCMP sample. As a result, a considerably low weight
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529 loss was detected in the first step compared to the untreated biomasses (Hai et al., 2022).

530 Furthermore, DCMP exhibited a weight loss of approximately 32.25% and 50% in the second

531 and third decomposition zones (150-225 °C and 225-440 °C), attributing to the decomposition

532 of lactose and sugars followed by fats and proteins in the carbon residue, respectively

533 (Bhushette & Annapure, 2017; Sunooj et al., 2011). The remaining residual mass content (ash)

534 was 15.25% at 900 °C.

535

536 3.5 Chemical characterization of spray-dried DCMP powder


537 The FT-IR spectra of DFE, carrier agent (MD), CMP, and DCMP are shown in Fig. 5. The

538 absorption peaks of DFE were observed at 3314 (broad), 1642, 1055, and 997 cm−1, attributed

539 to the stretching vibrations of the OH groups, C=C aromatic, COO−, and C–O of

540 carbohydrates, respectively (Deshwal et al., 2020). The FT-IR spectra of the CMP and DCMP

541 samples showed relatively similar peaks with intensity variations, demonstrating the

542 preservation of the important nutrients in the processed spray-dried DCMP. Milk is mainly

543 composed of fat, protein, and carbohydrates (lactose). Peaks at 2932, 2856, and 1743 were

544 attributed to the stretching vibrations of C-H, CH2, and C=O of fats present in DCMP (Wu et

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545 al., 2001). The characteristic peaks of C-O stretching vibrations in carbohydrates are displayed

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546 at wavelengths between 1250-800 cm-1. Strongly pronounced peaks in the range of 1000-1200

547
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cm−1 (1026 cm−1 ) are characteristic of lactose (Lei et al., 2010). The stretching vibration and
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548 the bending vibration peak in the range of 1500–1650 cm−1 correspond to the C=O of protein
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549 (amide I) and N–H of protein (amide II), respectively (Deshwal et al., 2020; Lei et al., 2010).
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550 The FT-IR spectrum of DCMP was in very close agreement with the published FT-IR spectra

551 obtained for spray-dried CMP (Deshwal et al., 2020; Habtegebriel, Wawire, et al., 2018).
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552 The nutritional analysis of DCMP obtained under the optimum operational conditions is

553 tabulated in Table 5. The table shows the measured quantities of macro-and micronutrients

554 present in DCMP together with the nutritional facts reported for commercial CMP. It is evident

555 that protein, fat, cholesterol, and minerals (Na, Fe, and Ca) in DCMP decreased drastically with

556 an increase in the total carbohydrate content owing to the addition of date sugar extract and

557 carrier agent to the feed solution before the spray-drying process. In addition, the fats profile

558 in DCMP sample showed reduced levels of saturated fats and good quantity of poly- and mono-

559 unsaturated fats (1.24 g/100g) which have beneficial effects such as loweing the risks of arterial

560 diseases, lowering plasma LDL cholesterol and total cholesterol (Bakry et al., 2021). The

561 cholestrol content in DCMP is 22.6 mg/100g, which is relatively low as compared to CMP
562 (132 mg/100g). Despite the reduction in some nutrients, the DCMP still showed a good

563 nutritional value. Similar results were found for the microencapsulation of curcumin with

564 coconut milk whey in the presence of gum arabic as a carrier agent (Adsare & Annapure, 2021).

565 The date sugar fortification caused an increase in fiber content from 0.00 to 0.81±0.069 g/100g.

566 Furthermore, the level of sugar content increased from 40.00 g/100g in CMP to 68.41±0.7

567 g/100g in DCMP, demonstrating the successful inclusion of reducing sugars (fructose and

568 glucose) and sucrose in CMP and the improvement in the sweetness level of camel milk.

569 Notably, the Sukkari dates (from which date sugar extract was prepared) contain 3.13% fiber,

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570 14.23% fructose, 15.83% glucose, 33.70% sucrose, and 0% lactose (Salem et al., 2017). This

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571 explains the significant increase in the fiber and total carbohydrates levels. Vitamins (A and C)

572
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were not detected in the DCMP sample due to the high processing temperature (160 °C) that
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573 causes the degradation of these vitamins, which has also been observed in other studies
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574 (Habtegebriel, Wawire, et al., 2018).


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575 [Table 5]
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576 The determination of the elements present in milk samples is important information that could
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577 help in minimizing the number of undernourished people in the world by recommending a

578 suitable diet based on their body needs. Elemental analysis using SEM/EDS revealed the

579 existence of the following elements: C, O, Na, P, Cl, K, Ca, Fe, Cu, and Rb (Fig. 5 (b)). The

580 results are in agreement with the elemental studies conducted on camel milk based on ICP-MS

581 and neutron activation analysis (Ahamad et al., 2017). Macronutrients such as Ca and K were

582 more abundant compared to Fe. These results were confirmed through nutritional analysis

583 results, demonstrating the excellent health benefits that DCMP offers, especially for people

584 suffering from hypocalcemia, anemia, and hypokalemia.


585 Considering the high nutritional value and other functional and morphological characteristics

586 such as thermal stability, high solubility, and easy handling due to unique morphology, Camel

587 milk fortified with date sugar powder could be used as is with the addition of water to prepare

588 a naturally sweet date-flavored liquid milk. DCMP can also be used in combination with other

589 products, such as coffee, to produce healthy sweet coffee with milk for latte enthusiasts and tea

590 to produce nutritious Karak. Additionally, DCMP could be used in many applications such as

591 beverages, ice creams, desserts, etc.

f
592 [Figure 5]

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593 3.6 Future prospects

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594
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Spray-drying techniques have long been used for different purposes, such as food preservation,
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595 drug encapsulation, flavoring, etc. Nevertheless, the production of high-value superfood
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596 products from fruits, vegetables, or plant waste is still an emerging topic that has recently
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597 gained attention and attraction. In this study, a highly nutritious camel milk powder enriched

598 with date sugar extract was produced and thoroughly studied. However, several other aspects
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599 must be investigated to ensure its commercial application on a larger scale. For insance, the
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600 effect of spray-drying conditions on the nutritional components of the final product and the

601 application of advanced drying technologies such as freeze-spray drying, which is known to

602 ensure the preservation of nutrients for food and nutraceutical applications. Certain powder

603 characteristics can be obtained by careful control of the drying rate and process conditions.

604 Thus, further optimization studies need to be performed with the goal of enhancing certain

605 powder properties through the multi-response approach. The kinetics of the Maillard reaction

606 in DCMP and the associated effect of the spray-drying conditions should be further investigated

607 to ensure the final quality of the powder obtained.

608
609 4. Conclusion

610 To address the urgent need for innovative, highly nutritious products from unused food

611 resources, camel milk powder encapsulation with date sugar was explored using spray-drying

612 techniques with minimal addition of maltodextrin as a carrier agent. Operating conditions were

613 optimized to maximize the overall product recovery and temperature gradient using response

614 surface methodology with a central composite design. The most effective process parameters

615 for powder yield were air inlet temperature and carrier agent concentration. A maximum

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616 overall yield of 55 wt./wt.% was achieved at 160 °C, 7 mL/min, and an MD concentration of

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617 3.1 wt./v%. The results of the spray-dried DCMP product prepared under optimized conditions

r
618 -p
showed relatively good morphological characteristics such as small particle size of 1.2-27.7

619 μm, smooth surface, amorphous nature, and spherical shape, which facilitates the packaging
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620 and processing of the powder and improves the functional properties of the powder. In addition,
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621 the good thermal stability and nutritional value of DCMP (higher fiber conent 0.81g/100g),
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622 lower cholestrol content (22.6 mg/100g), and good quantity of poly- and mono-unsaturated fats
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623 (1.24 g/100g)) makes it an excellent dietary supplement.


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624

625 Acknowledgement

626 This work is supported by the project grant CIRA-2019-028 under the Competitive Internal

627 Research Award scheme of Khalifa University, UAE.

628

629 Declaration of competing interest

630 Authors declare that there are no relevant financial or non-financial competing interests to

631 report.
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862
Tables

Table 1. Coded and un-coded levels of the studied spray-drying factors and the corresponding
response values of the spray-dried DCMP.
Factors Response Recorded
values
Coded values Experimental values
Run 𝑻𝒊𝒏𝒍𝒆𝒕 , Feed flow MD conc., 𝑻𝒊𝒏𝒍𝒆𝒕 , °C Feed MD conc., 𝒀𝒐 , % 𝑻𝒐𝒖𝒕𝒍𝒆𝒕 , °C ΔT,
°C (X1) rate, w/v % (X3) (X1) flowrate, w/v % (X3) (Y1) (Y2) °C
mL/min mL/min
(X2) (X2)
1 -1 -1 -1 120 2 1.15 6.4 83.7 36.3
2 1 -1 -1 160 2 1.15 44.9 107.8 52.2
3 -1 1 -1 120 10 1.15 21.2 78.5 41.5
4 1 1 -1 160 10 1.15 26.6 92 68.0

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5 -1 -1 1 120 2 4.6 12.8 84.5 35.5
6 1 -1 1 160 2 4.6 46.9 103 57.0
7 -1 1 1 120 10 4.6 40.3 73 47.0

r
8 1 1 1 160 10 4.6 32 99.3 60.7
9
10
-1
1
0
0
0
0
120
160
-p 6
6
2.875
2.875
39
52.8
81.5
103.3
38.5
56.7
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11 0 -1 0 140 2 2.875 23.9 89.8 50.2
12 0 1 0 140 10 2.875 53.5 90.5 49.5
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13 0 0 -1 140 6 1.15 36.8 95.3 44.7


14 0 0 1 140 6 4.6 50 98.8 41.2
15 0 0 0 140 6 2.875 57 99.7 40.3
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16 0 0 0 140 6 2.875 55.1 89.8 50.2


17 0 0 0 140 6 2.875 47.5 87.3 52.7
18 0 0 0 140 6 2.875 49.7 88.6 51.4
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19 0 0 0 140 6 2.875 52.3 95.1 45.0


20 0 0 0 140 6 2.875 56.6 97.7 42.3
Jo
Table 2. ANOVA for overall yield and outlet air temperature response surface functions on
the effect of operating conditions (air inlet temperature, feed flow rate, and MD concentration).

𝒀𝒐 , % (Y1) 𝑻𝒐𝒖𝒕𝒍𝒆𝒕 , °C (Y2)


Model S S
Linear terms
X1 S S
X2 NS S
X3 S NS
Interaction terms
X1X2 S NS
X1X3 NS NS
X2X3 NS NS
Quadratic terms
X12 NS NS

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X22 S NS

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X32 NS NS
Lack-of-Fit NS NS

r
R2 90.3 85.3
Adjusted R2
C.V (%)
-p 81.6
6.5
72.1
4.8
re
X1: Inlet air temperature, X2: Feed flow rate, X3:Carrier agent (MD) concentration; Yo: overall yield, Toutlet:
Outlet air temperature, S: significant (P<0.05), and NS: not significant (P>0.05).
lP
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Jo
Table 3. Predicted and experimental values of the model variables and responses at the
optimum point of spray-drying operation for date sugar encapsulated camel milk powder.
𝑻𝒊𝒏𝒍𝒆𝒕 , °C Feed flow rate, MD conc., 𝒀𝒐 , % ΔT
(X1) mL/min (X2) w/v % (X3) (Y1)

Predicted 160 6.93 3.1 54.11 59.02


Experimental 160 7.0 3.1 55.17±0.74 59.88±1.11

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lP
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Table 4. Functional properties of spray-dried DFE-fortified camel milk powder (DCMP).

CMP DCMP
Functional Properties Free bulk ρ (FBD) (g/L) 460±10 400±10
Tapped bulk ρ (TBD) (g/L) 550±20 560±20
CI 17.03±0.51 29.23±1.09
Flow-ability Fair Poor
HR 1.21±0.01 1.41±0.02
Cohesiveness Intermediate High
Moisture content (%) 2.40±0.71 3.63±0.01
Solubility (%) 77.52±0.42 77.26±0.03
Color properties L* 72.48±1.23 77.47±0.69
a* 8.53±0.15 -1.49±0.04
b* 27.86±0.01 9.00±0.04

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c* 29.1±0.04 9.13±0.05

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h* 72.98±0.28 99.36±0.18

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-p
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Table. 5. Nutritional analysis of CMP and DCMP.

No. TEST UNIT DCMP CMP*


1 Energy (Calories) kJ/ 100g 1568.25±2.26 2058
2 Total Fat g/100g 3.38±0.09 26
3 Saturated Fat g/100g 2.12±0.1 18
4 Polyunsaturated Fat g/100g 0.12±0.005 n.r
5 Monounsaturated Fat g/100g 1.12±0.04 n.r
6 Cholesterol mg/100g 22.62±0.35 132
7 Sodium mg/100g 395.73±41.19 658
8 Potassium g/100g 1.66±0.17 1.76
9 Total Carbohydrates g/100g 70.56±0.17 40
10 Dietary Fiber g/100g 0.81±0.069 0

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11 Total Sugar (Glucose, g/100g 68.41±0.7 40
Fructose, Sucrose, Lactose)
12 Protein g/100g 15.54±0.14 26

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14
Vitamin A
Vitamin C
-p mg/100g
mg/100g
n.d
n.d
0.12
23
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15 Calcium mg/100g 544.47±65.09 902
16 Iron mg/100g 0.51±0.06 0.90
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* The nutritional facts of the commercial camel milk powder, nr: not reported, n.d: not detected.
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Figures’ captions:
Fig. 1. Schematic representation of DCMP production using spray-drying technique.
Fig. 2. Single factor effect on the studied responses, (a) effect of varying the air inlet
temperature on the overall yield, (b) effect of varying the air inlet temperature on the outlet air
temperature and ΔT, (c) effect of varying the feed flow rate on the overall yield, (d) effect of
varying the feed flow rate on the outlet air temperature and ΔT, (e) effect of varying the MD
concentration on the overall yield, (f) effect of varying the MD concentration on the outlet air
temperature and ΔT.
Fig 3: The effect of spray-drying operating conditions on the overall yield. Contour plots of
(a) Yo vs. feed flow rate and air inlet temperature, (b) Yo vs. MD concentration and inlet
temperature, (c) Yo vs. MD concentration and feed flow rate; surface plots of (d) Yo vs. feed
flow rate and air inlet temperature, (e) Yo vs. MD concentration and inlet temperature, (f) Yo
vs. MD concentration and feed flow rate.

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Fig. 4. SEM images of (a-c) commercially available CMP and (d-f) date sugar fortified camel
milk spray-dried powder (DCMP) obtained under optimized operating conditions at 500x,
1000x, and 5000x.

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Fig. 5. (a) FT-IR spectra of Date Fruit Extract (DFE), Maltodextrin (MD), Camel Milk
Powder (CMP), and Date sugar fortified CMP (DCMP), (b) elemental analysis of DCMP
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using SEM-EDX.
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Figures:

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Highlights

• Production of date sugar encapsulated camel milk powder (DCMP) using spray dryer.
• Optimization of spray drying parameters for maximizing DCMP yield.
• Inlet air temperature and carrier agent concentration increased the powder yield.
• DCMP powder showed improved functional properties and thermal stability.
• Date sugar fortified camel milk powder exhibited high nutritional values.

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Declaration of Interest Statement

All the authors of the research article declare that the submitted manuscript has been read by
everyone and there is no conflict of interest regarding the publication of this paper.

Thanking you,

Sincerely yours,

of
Prof. Fawzi Banat
(Corresponding Author)

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