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Production of encapsulated (25R)-Spirost-5-en-3β-ol powder with composite coating material

and its characterization

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Prajya Arya* and Pradyuman Kumar

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Department of Food Engineering and Technology
Sant Longowal Institute of Engineering and Technology
Longowal Punjab 148106, INDIA
prajyaarya27@gmail.com & pradyuman2002@hotmail.com

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+91-9958304721, +91-9417321580

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Corresponding author*
Running title: (25R)-Spirost-5-en-3β-ol powder produced from composite wall materials.

ORCID er
Prajya Arya: https://orcid.org/0000-0002-3847-5074
Pradyuman Kumar: https://orcid.org/0000-0002-0690-9800
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This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4333501
1. Introduction

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With the growing trend of a new lifestyle, the incidence of chronic diseases is becoming more
evident and with contempt for upcoming advancements in treatment methods, synthetic

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medication is kept on grating the side effects of life-threatening diseases [1]. Bioactive
compounds and phytochemicals are taking a loop in the current medicine [2]. (25R)-Spirost-5-
en-3β-ol (diosgenin) is the steroidal compound found in Trigonella foenum graecum [3] that
occurred in form of glycoside [4]. Diosgenin is quite recognized for its promising health

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benefits including atherosclerosis [5], cardiovascular tissues protection [6], inhibits ER stress-
induced inflammation in aorta via iRhom2/TACE mediated signaling pathways [7],

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hypolipidemia [8], a neurological disorder [9], protect alveolar bone loss [10], prevention of
fatty liver disease [11], nephroprotective potential [12] Mishra et al., 2021), maintaining gut-
microbiota hypersensitivity [13], improve cognitive functioning [14], skin diseases [15],
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gastroprotective properties [16] and many more. Diosgenin crucial role in maintaining the
proper cellular mechanism and must aid in the utilization of silent deadly diseases like cancer
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[17] and diabetes [18].

Diosgenin is arriving at the verge of validating and expanding comprehensive knowledge and
proving itself as a novel drug for chronic diseases due to its mechanistic pathways against
manifold illnesses [19]. Diosgenin helps in the suppression of cancer cells and other metabolic
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diseases by triggering programmed cell death and inducing apoptosis of infected cells [17].

Scorn of such health-promising benefits of diosgenin, its utilization, consumption, and delivery
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as a product is remarkably less due to its bitter taste and astringent flavour when extracted from
fenugreek seed [20]. So, to avail of the benefits of diosgenin appropriately, there must be a way
for its better delivery and consumption. The current research rivets over the spray drying of
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fenugreek’s diosgenin with different drying aids. The concept of spray drying facilitates the
conversion of liquid feed into a powder that causes enhancement of the shelf of the bioactive
compound and makes them deliverable to the target sites [21]. The spray drying of diosgenin
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could provide new ways to the food and pharmaceutical industries as its thermal stability,
decomposition initiation, and decomposition end at 213.9 °C, 276.1 °C, and 435.6 °C
respectively [22] which provides proficient thermal stability to the diosgenin during spray
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drying. From the recent market trend, there is epic gain in nutraceutical food products which

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are loaded with microencapsulated microcapsules of various bioactive compounds that
provides wheels to the pharmaceutical and food market to reach 15.6 USD by 2026 [23].

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There is very less study conducted with diosgenin and different wall materials to produce an
edible food grade spray dried diosgenin powder. The study conducted with diosgenin in respect

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of drug delivery observed the anticancer effect of diosgenin [24], but not much in favor of food
grade substances and products. This current research paper focuses on the production of spray
dried encapsulated (25R)-Spirost-5-en-3β-ol (diosgenin) powder with two different wall
materials alone or in combination and studying their properties proven with aid of DSC and

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FTIR analysis, it could be a better source of providing health beneficial properties of diosgenin
to the human health.

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2. Experimental section
2.1. Feed preparation for spray drying of diosgenin
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The diosgenin used for spray drying was extracted by ultrasound assisted extraction method as
per Arya and Kumar [20]. The diosgenin was added in varying percentages ranging from 0.1-
0.5 % with maltodextrin (MD; DE-20) and whey protein concentrate (WPC; 80 % concentrate)
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and was used as different wall materials for microencapsulation. The wall materials were
procured from Loba Chemie, Pvt. Ltd, Mumbai and Mahaan Protein Ltd, New Delhi,
respectively. The wall material solutions were prepared separately by dissolving MD, and WPC
as 20 %, and 10 % respectively in distilled water at 40 °C, followed by the addition of diosgenin
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in varying percentages and the final volume was made up to 500 mL. Each feed was separately
mixed with aid of a magnetic stirrer for 40 min at 35 °C to attain a lump-free slurry recognized
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as feed. The feed was fed into a laboratory scale spray dryer (SM Scientech, Kolkata, India)
with co-current airflow. The inlet air temperature (IAT:160°C) and feed flow rate (FFR: 400
mL/h) were kept constants for all the samples. The spray dried diosgenin powder was kept in
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zipped bags that were placed in an airtight container at 4 °C for further studies. The samples
were coded as shown in Table 1 for MD and WPC.

2.2. Powder recovery


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The yield of encapsulated diosgenin powder was determined by the mass of total solids in
powder in ratio to total solids in feed solution [25] and calculated by equation (1).
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Total weight of resulting powder on a dry basis


𝑃𝑜𝑤𝑑𝑒𝑟 𝑅𝑒𝑐𝑜𝑣𝑒𝑟𝑦 (%) = 𝑇𝑜𝑡𝑎𝑙 𝑠𝑜𝑙𝑖𝑑 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 𝑖𝑛 𝑓𝑒𝑒𝑑
∗ 100 (1)

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2.3. Powder properties
2.3.1. Moisture content

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For the measurement of moisture content in diosgenin powder, AOAC method 976.05 was
followed. The accurately weighed 5 g samples were placed in pre-weighed empty petri-dishes

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in a stifling air oven at a temperature of 105±5 °C for 4 h [26]. The moisture content was
estimated by following equation (2)

(𝑊2 ‒ W)
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 = (𝑊 ∗ 100 (2)
1 ‒ W)

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Where W= weight of empty petri-dish; W1= weight of petri dish with sample before drying;
W2= weight of petri-dish with sample after drying

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2.3.2. Water activity

The measurement of water activity was analysed using a pre-calibrated water activity meter
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(HYGROLAB, Rotronic, Cole-Parmer), all the data was recorded in triplicates and at room
temperatures [27].
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2.3.3. Bulk and tapped density

The bulk and tapped density of the powdered were measured by weighing 5 g of powdered
sample into a calibrated measuring cylinder and observing the reading of occupied volume
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from powder. The tapped density was determined by measuring the volume of the graduated
cylinder by tapping three hundred times until no further change in powder volume was
observed [28].
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2.3.4. Flowability (compressibility index & hausner ratio)

The flowability of the powder was measured in terms of Carr’s index [29] and Hausner ratio
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[30], and the range of flowability is expressed in Table 2 and calculated by the respective
following equation (3) and (4).

(Tapped Density ‒ Bulk Density )


𝐶𝑎𝑟𝑟'𝑠𝐼𝑛𝑑𝑒𝑥(%) = (3)
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Tapped Density
∗ 100

Tapped Density
𝐻𝑎𝑢𝑠𝑛𝑒𝑟 𝑅𝑎𝑡𝑖𝑜 = Bulk Density
(4)
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2.3.5. Hygroscopicity

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The hygroscopicity of spray dried diosgenin powder was calculated by observing the moisture
absorption capacity of the powder by exposing it to the relative humidity of 75 % with sodium

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chloride. Accurately weighed 0.5 g samples were placed in pre-weighed watch glasses and kept
in a desiccator containing a saturated solution of sodium chloride at room temperature. The
change in weight of the sample was observed after seven days and all the samples were

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determined in triplicate [31]. The hygroscopicity of the powdered sample was calculated under
the given equation (5).

Weight gain in sample


𝐻𝑦𝑔𝑟𝑜𝑠𝑐𝑜𝑝𝑖𝑐𝑖𝑡𝑦 (%) = Weight of the sample
∗ 100 (5)

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2.3.6. Encapsulation efficiency

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The spray dried diosgenin powder was studied for encapsulation efficiency [31] and it was
calculated using under given equation (6).

Total diosgenin ‒ Surface diosgenin


𝐸𝑛𝑐𝑎𝑝𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 =
er Total diosgenin
∗ 100 (6)

2.3.7. Solubility
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The one-gram spray dried diosgenin powder dissolved in 10 mL of distilling water at room
temperature. The mixture was vortexed for 30 sec and centrifuged at 6000rpm for 10 min. The
supernatant was poured into pre-weighed and pre-dried petri-dishes and dried at 105±5°C until
moisture was removed from the petri-dishes [32]. The solubility was analysed by the weight
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change of the remaining solids as shown in equation (7).

𝑊𝑑𝑠
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𝑊𝑎𝑡𝑒𝑟 𝑠𝑜𝑙𝑢𝑏𝑖𝑙𝑖𝑡𝑦 (𝑤𝑠)% = 𝑊𝑆


∗ 100 (7)

Where Ws%= water solubility percent; Wds= weight of dissolved solids in supernatant; Ws=
weight of the sample.
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2.3.8. Degree of caking

The diosgenin powder was analysed for the degree of caking followed by hygroscopicity. The
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moisture-gained samples were kept in a stifling air oven at 80°C for a duration of 4 h. The
samples were kept in a glass desiccator until cooled and the weight of the powder sample was
measured. The sample was sieved out from five hundred µm size followed by manual shaking
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of the sieve [33] The degree of caking was analysed by observing the weight of the sample left
in the sieve [34] and calculated by following equation (8).

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Amount of powder remained on the sieve after sieving
𝐷𝑒𝑔𝑟𝑒𝑒 𝑜𝑓 𝐶𝑎𝑘𝑖𝑛𝑔 (%) = Amount of powder used in sieving
∗ 100 (8)

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2.3.9. Color

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The powdered samples were kept in a small transparent airtight zipper pouch and allowed for
maximum exposure at the scanning part of the CIELAB color system [35]. Color parameters
of the powdered samples were measured in a colorimeter (CH-8105 Regensdorf, Gretag

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Macbeth, Switzerland) and results were expressed in form of L, a*, and b* values.

2.3.10. Particle size analysis

The particle size analysis of diosgenin powder prepared from different wall materials was
analysed by using a laser diffraction particle size analyser (SALD 2300 Shimadzu, U.S.A.)

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[36]. The span index was applied to check the polydispersity of the particle size as mentioned

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in equation (9)

𝐷90 ‒ 𝐷10
𝑆𝑝𝑎𝑛 = 𝐷50
(9)
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2.3.11. Differential scanning colorimetry

The thermal stability of diosgenin powder was analysed using differential scanning colorimetry
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(DSC 4000, Perkin Elmer, USA) equipped with a thermal analysing station by observing glass
transition temperature (Tg). An empty aluminium pan was used to analyse the samples. The
aluminium pan was sealed with a lid and heated from 0 to 250 °C and at a rate of 20 °C per
min. the thermal scanning of samples was recorded in form of onset, midpoint, and end points
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of Tg [37].

2.3.12. Fourier transformation infrared spectroscopy


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Diosgenin powder was analysed for observing the presence of different bonds that form during
spray drying. The FIR spectrum was studied with aid of the FTIR spectrum (L1600300
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Spectrum Two-LIT-a FTIR, UK) and studied for pure samples of maltodextrin, whey protein
concentrates and powder prepared from these wall materials [38].

2.3.13. Statistical analysis


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The statistical analysis of the selected properties was performed for analysis of variance
(ANOVA) using software JMP® 12.1.0 (SAS institute Inc., NC, USA). Each test was
conducted in triplicates. ANOVA was conducted with Tukey’s test to identify significant
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differences at (p < 0.05) with a 95 % level of confidence.

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3. Results and discussion
3.1. Powder recovery

During spray drying, powder recovery always has a beaut role in predicting the significance of

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an effective drying process. In this study, powder recovery was observed for powder from MD,
and WPC that were coded as (A-E), and (F-J). The range of powder recovery varied for (A-E),
and (F-J), with a significant difference (p<0.05) (33.69 - 54.77 %), and (51.53 - 64.69 %) as
shown in Fig. 1. The effect of carrier agents was observed over powder yield that depicted the

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lowest recovery with MD and highest recovery WPC. The highest recovery of spray dried

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diosgenin powder was observed in case of WPC as compared to MD due to the higher content
of protein and surface activity which cause the foaming interface of the feed mixture. The
variation in powder yields is due to different carrier agents caused by change in molecular
weight of MD and WPC that is affected by their glass transition temperature. This aids in the
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reduction of stickiness with the drying chamber wall during drying by forming a layer over
feed particles [39]. The yield of powder is related to the glass transition temperature of carrier
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agents that cause agglomeration and stickiness in the drying chamber thus causing less powder
production [40]. The current study showed relevance to studies conducted over tomato pulp
powder that yielded powder in the range of 36.62 to 65.86 % [41]. The study of beetroot juice
powder production with the spray drying technique yielded in range of 52.1 to 90 % with
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different carrier agents [42]. The preparation of honey powder with maltodextrin, gum arabic,
and whey protein concentrate by spray drying ranged from 53.45 to 65.10 % [43]. The spray
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drying of tamarind pulp powder ranged from 9.35 to 70.04 % by using maltodextrin and soy
protein isolates [44]. The spry dried powder of goldenberry juice yielded in the range of 49.7
and 67.2 % [31].
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3.2. Moisture Content

The spray dried diosgenin powder with MD, and WPC revealed moisture content in range of
(1.94 - 3.78 %), and (1.85 - 3.91 %), with a significant difference (p<0.05) for (A-E), and (F-
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J). The observed moisture content is less than 5.25 % which ensures microbial safety of the
powder [45]. The small variation in the moisture content of powder produced is due to the
branched structure that alters the moisture absorption from the nearby environment [45]. The
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moisture content in WPC powder is more as compared to MD due to the formation of a layer
over liquid particles that hinder water evaporation during drying [42]. The spray dried lactose

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powder produced by soluble soybean polysaccharide was evaluated for moisture content that
ranged from 2.08-4.98 g/100g dry basis in support of the current study [46]. The moisture

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content of cloudy beetroot juice powder ranged from 3.5-4.1 % [42]. The moisture content of
the tamarind pulp powder with WPC ranged in a similar range due to the high concentration of
WPC causing much higher water retention [47]. There was another study conducted for

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tamarind pulp powder with soy protein isolate depicted an increment in protein content in the
feed, and an increase in moisture content of spray dried powder was observed [44].
Theoretically, it was observed that the moisture content of spray dried powder was not more
than 5 %, so the present study conducted produced satisfactory results [48].

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3.3. Water activity

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The water activity (aw) is the measure of the degree of available water in food which is
measured by observing the ratio of the equilibrium water pressure of the sample to the
equilibrium vapor pressure of the pure water at the same temperature [49,50]. The water
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activity of spray dried diosgenin powder ranged from (0.397-0.430), and (0.413-0.498), with a
significant difference (p<0.05) for (A-E), and (F-J). The moderate range of aw was produced
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from spray dried diosgenin powder with 0.3 % diosgenin feed composition as compared with
other feed compositions due to its hygroscopic nature which is reflected in the spray dried
powder. The variation in aw of the spray dried powder was observed to be maximum in WPC
and followed by MD. The aw of the date powder was in the range of 0.23 to 0.28 depicting the
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effect of high MD concentration over the aw of the date powder sample [27]. This study was
correlated with the date powder produced by the oven drying method yielded an aw of 0.297 to
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0.334 which produces powder with a high aw. The effect of the following factors was observed
aw by monitoring carrier agent amounts, processing type, and raw material to be processed [51].
The current study revealed comparable results with persimmon powder produced by spray
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drying had an aw of 0.195 - 0.205 [52], and spray dried raisin with MD had an aw of 0.46 [53].

3.4. Bulk and Tapped Density

The bulk density of spray dried diosgenin powder ranged from (0.414-0.509 g/mL), and (0.209-
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0.225 g/mL), for (A-E), and (F-J) as shown in Table 3. The bulk density is affected by the
atomization pressure and inlet air temperature [54]. Bulk density is the measure of powder
characteristics that are significantly affected by particle size and porosity. during the spray
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drying process, there is the formation of vapor impermeable film over the atomized feed droplet
that causes bubble formation by the expansion of the droplet. The fluctuation in temperature

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causes an effect on bulk density as during high inlet air temperature, bulk density reduces
imparting a more fragile, fragmented, and porous structure which is commonly called the

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ballooning and puffing effect [55].

Tapped density is the volume of mass occupied inside a closed chamber by a sample doing the

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tapping to remove trapped air inside intermolecular spaces. The tapped density depicts the
utmost packaging of spray dried powder under the influence of well-defined boundaries when
applied to external forces [56]. The tapped density of diosgenin powder ranged from (7.80-
9.30), and (16.23-18.30) with a significant difference (p<0.05) for (A-E), and (F-J) as shown

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in Table 3. The current study has similarities with the tapped density of durian fruit seed by
spray drying ranging from 0.199-0.258 g/mL [56], and 551.72-782.50 kg/m3 of sweetened

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yogurt powder [54].

3.5. Flowability
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Flowability is the measure of the Carr’s index and Hausner ratio that aids in predicting the flow
behavior of the powder as shown in Table 2. It indicates that poor to moderate flow results
from finer particles to interparticle cohesiveness which acts as a constraint that needs to be
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monitored in powder flow crucial properties [57]. The Carr’s index and Hausner ration of
diosgenin powder ranged from (20.81-24.75 %; 1.24-1.34), and (22.32-31.49 %; 1.26-1.37),
with a significant difference (p<0.05) for (A-E), (F-J). The WPC addition tends to have more
entrapment of air during drying which hinders the flow properties of powder by suppressing
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the stickiness of particles by the formation of a thin, skinny layer [58]. The CI and HR of
sapodilla pulp powder produced by spray drying ranged from 53.2- 59.9 and 2.14-2.50 as
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shown in the current conducted study [59]. The study has a similarity with spray drying of
vitamin E microencapsulation with MD and WPI that ranged from 0.42-0.61 g/cm3 [60].

3.6. Hygroscopicity
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The concept of hygroscopicity was introduced to observe and study the ability of the powder
to absorb the water from a nearby natural environment that hinders storage properties of the
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powder and leads to acts as plasticizer and clumping followed by stickiness [61]. The
hygroscopicity of spray dried diosgenin powder is represented in Table 3 with the following
range from (10.98-14.21 %), and (9.53-11.42 %) with a significant difference (p<0.05) for (A-
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E), and (F-J). The hygroscopicity of spray dried diosgenin powder was affected by the moisture
gaining nature of extracted diosgenin. Among different feed compositions, 0.3 % diosgenin
produced an acceptable range of hygroscopicity of the powder. The powder prepared from

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MD had much high hygroscopicity as compared to WPC that revealing powder stability during
shelf-life storage. The relation of moisture content to hygroscopicity was analysed as it

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revealed about the less amount of water present in powder, it could be more hygroscopic due
to the difference between dried powder and moisture present in the surrounding environment
that imparts a pressure that acts as a driving force for the moisture gain in less moisture

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containing powders. The current study is in support of the research conducted for beetroot juice
powder that also observed similar effects [62]. The effect of carrier agents was observed for
the hygroscopicity of beetroot juice concentrate which showed MD powder had higher
hygroscopicity as compared to other carrier agents used in powder production [42]. The

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hygroscopicity of spray dried powders affected by the particle size, the smaller the particle size,

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the higher would be the hygroscopicity of powder [35]. The particle size of the current study
validates the support for hygroscopicity and particle size.

3.7. Encapsulation efficiency er


Encapsulation is a method of entrapment of bioactive substances into suitable wall material
composed of various edible food grades corporeal [63]. Encapsulation produces small droplets
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of size 1-1000 µm that coat bioactive compounds and protects them from several
environmental factors like oxygen, light, pH, chemical interactions, and moisture [64]. The
encapsulation efficiency of spray dried diosgenin powder varied from (43.72-79.91 %) and
(60.06-72.75 %) with a significant difference (p<0.05) for (A-E), and (F-J) as shown in Fig. 1.
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The effect of wall material was observed over the encapsulation efficacy that depicted
minimum with MD, followed by WPC. The variation was observed due to the altering quantity
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of diosgenin that hinders encapsulation efficiency. The MD and WPC also yielded better
encapsulation efficiency due to a high number of dry solids in the feed preparations [65, 66].
The combined effect of wall materials and diosgenin revealed the hydrophobic effect in an
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aqueous solution that captivate molecules and produced better outcomes. This could be
supported by the fact that the formation of polysaccharide and protein-rich complex leads to
better encapsulation efficiency as compared to the only type of wall materials [67]. The current
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study was in similarity with the encapsulation efficiency of spray dried probiotic powder at
96.50 % [68], goldenberry at 77.2 % [31], β-carotene with alginate and chitosan was 37.7 %
and 54.7 % respectively [69].
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3.8. Solubility

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The diosgenin spray dried powder solubility is shown in Fig. 1. The variation in solubility was
observed for (A-E) and (F-J) with a significant difference (p<0.05) as (81.02-84.81 %) and

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(79.86-88.86 %). The solubility of spray dried diosgenin powder was affected by the extracted
diosgenin solubility as it aids in solubilizing wall materials during the process. The 0.3 %
diosgenin produced the best solubility as compared with other feed mixtures as shown in Fig.1.

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The sample prepared with MD showed higher solubility due to high dissolution in water [33].
The solubility of spray dried mango powder ranged up to 90 % as studied by [32]. The solubility
of pomegranate juice powder was 84.93 % which also supported the present study [70]. The
effect of carrier agents showed that the solubility of spray dried powders could be either

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suppressed or enhanced [71]. The study conducted for sumac extract powder also depicted high

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solubility for the maltodextrin-prepared spray dried powders [72], and the preparation of
acerola powder was in the similarity of above-mentioned results [73]. The solubility of powders
is at times hindered by the temperature of dissolving water causing a quick sink of large powder
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particles while small particle float over the surface [74]. The similarity was analysed for orange
juice powder [75] and watermelon juice powders [76] with a cause of formation of a protective
surface layer due to high inlet temperatures that preclude water molecules from diffusing via
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particles which dwindle the wettability of particles and cause a reduction in the dissolution of
spray dried food powders [70].

3.9. Degree of caking


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The degree of caking of spray dried powders depicts unfavourable reactions which transform
powder particles by agglomerating them and making them sticky that causing a loss of
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functional properties of powders [77]. The diosgenin spray dried powder degree of caking
ranged from (20.81-24.75 %), and (22.32-31.49 %) with a significant difference (p<0.05) for
(A-E), and (F-J), as shown in Table 3. The acceptable range of degree of caking of spray dried
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diosgenin powder was observed with 0.3 % diosgenin in the feed mixture as compared with
other feed compositions. The rich hygroscopic nature of extracted diosgenin that quickly
absorbs moisture from a nearby environment contributes to the gamy degree of caking. The
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variation in the degree of caking was observed due to polysaccharide and protein usage in wall
material that hinders the moisture uptake from nearby environment. The current study had a
high degree of caking as of the high molecular weight of core and wall material and varying
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diosgenin concentrations in the feed. Degree of caking forms a layer of moisture over particles
that alters their structural properties and makes particles sticky by forming a liquid bridge in
the intermolecular spaces of the powder particles [26]. The present show relevance of the

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degree of caking analysed for an instant coffee powder that ranged from 9-34 % [34], and spray
dried yoghurt powder degree of caking was observed to be 30.32 % that produce supportive

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data with present study [78].

3.10. Color

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Color is a majorly specific property regarding spray dried food powders that pronounce the
acceptance of end products. The color properties of spray dried diosgenin powder are revealed
in Table 4 with a caption of L*, a*, b*, hue, and chroma performed by a CIE color
spectrophotometer. The analysis was performed to observe as L* indicates brightness to

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blackness (0 to 100), a* indicates green (-) to red (+), and b* indicates blue (-) to yellow (+)

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[79]. The range of color parameters varied for L*, a*, b*, chroma, and hue as shown in Table
4. The variation in color properties of diosgenin powder was due to different wall materials as
L*, and b* values are high as compared to a* values. The color variation was observed in spray
dried diosgenin powder due to the amount variation of diosgenin and wall materials used. The
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most acceptable color was produced and observed from 0.3 % diosgenin used in encapsulation
with MD, and WPC as shown in Table 4. The tint of whitish to pale yellow color is the proper
pe
indication of the addition of diosgenin which was amber yellow. The MD and WPC impart
bright white and tint yellowish color that alters final powder color values that are hindered by
browning reaction occurred during spray drying followed by caramelization and Maillard
reaction that triggered by the different sugar content of wall materials [80]. The color
ot

parameters are affected by soluble solid content, and the concentration of the core and carrier
agents required to be encapsulated by spray drying [81]. The current study has shown that
tn

equivalent results found with the sea buckthorn juice powder prepared with MD revealed L*
89.26, a* -1.26, b* 36.77, chroma 36.79, hue 91.88 [79]. The spray drying of pineapple powder
was having L*, a*, and b* as 97.40, -0.25, and 1.59 respectively [82]. The effect of wall
rin

material also alters L*, a*, and b* values as observed by [76] while preparing watermelon spray
dried powder. It occurs due to dilution of the core material while preparing the feed by
producing sapodilla powder with MD [83].
ep

3.11. Particle size analysis

The particle size analysis of spray dried powder always leads to a major character as it
maintains the different linked properties. The spray dried diosgenin powder is shown in Table
Pr

4 and depicted in form of D10, D50, D90, and span values. The effect of wall material and core
material hinders the particle size during atomization which decides the final droplet size and

This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4333501
causes fineness of the powder, enhanced aggregation, and fracture resistance of the powder
particles [84]. The powder particle showed an acceptable range of D10, D50, and D90 depicting

ed
powder was super fine. The powder particle size is impacted by solubility as smaller particles
would cause higher solubility and the current study supports the solubility and particle size data
[85]. The spray dried diosgenin powder revealed an acceptable range of diosgenin particles

iew
produced. The study had similarities with the microcapsules prepared with d-limonene and MD
and WPC yielded particle sizes of 1.30-3.65 % [86]. The spray drying of bioactive and volatile
compounds of smoke powder food flavouring produced 96.1 µm [87].

v
3.12. Differential scanning colorimetry

re
The glass transition of diosgenin powder was shown in Fig. 2 for the most suited and selected
samples of diosgenin powder with different wall materials. The samples were coded as C, and
H, for MD, and WPC. These selected samples represented the other utmost properties of
diosgenin powder. The thermal profiling depicts the temperature stability with onset
er
temperature, midpoint temperature, and end-set temperature for C (26.97, 32.24, and 34.85°C),
and H (83.57, 81.61, 78.63°C). The temperature range of C, and H, samples predicted better
pe
thermal stability as provided by both drying aid to their respective samples. The DSC curves
of diosgenin with distinct types of drying aids MD, and WPC revealed that 0.3 % diosgenin
showed an exothermic peak between 50 and 150 °C, depicting about thermal denaturation of
the selected samples. The uniformity was observed in all three samples with an insignificant
ot

change in each peak. The binding of diosgenin with MD and WPC enhances the thermal
stability of the spray dried powders. This study revealed the interaction of diosgenin with wall
tn

material and altering the glass transition temperatures as shown in Fig. 2. The study has
similarities with the spray drying of citrus flavonoids with gum arabic and MD revealing glass
transition temperatures ranging from 50 to 200 °C that indicate moisture loss and denaturation
rin

of the powdered samples. The citrus peel extracts flavonoid denaturation and glass temperature
depicted range from 120 to 240 °C [88]. The glass transition profile of lactose permeates
showed a range from 85-95 °C of thermal stability [89].
ep

3.13. Fourier transmission infrared spectroscopy

The powder was analysed for observing functional and structural bonds that were affected
during drying and preparation with different carried agents, followed by observing wavelength
Pr

in transmittance (%T) [18]. The FTIR spectrum of spray dried diosgenin powder was observed
for most appropriate samples of drying experiments (C, and H) and revealed presence of bands

This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4333501
for C (3272.95, 1359.57, 1149.68, 1078.18.1019.92, 847.73,632.81 cm-1), and H (3267.07,
1629.95, 1537.66, 1076.21, 650.76, 627.48,620.29, 612.66 cm-1) is shown in Fig. 3. The

ed
presence of bands was observed in the range of 3260-3280 revealing OH stretching with a weak
and broad peak. This is followed by 1650-1600 showing with C=C bond linked with conjugated
alkene with medium strength, 1350-1300 with S=O bond linked with sulfonamide with high

iew
strength, 1150-1085 contain C-O stretching with aliphatic ether and high strength, and 730-665
contain C=C alkene bonds with high strength. The effect of wall material MD, and WPC, also
showed the presence of bonds like C-C, C-O, and C-H that occurred due to interaction of
diosgenin with respective wall materials like the presence of amide II group at 1500-1600 cm-

v
1 wavelength showed interactions of diosgenin with WPC [66]. The current study showed

re
similarity with spray dried honey powder having bands occurrence at 3650-3000 cm-1 (OH
stretching region), 3000-2800 cm-1 for sugar C-H skeleton, 1715 cm-1 with carbonyl C=O
functionalities present in ketone and glucose [90, 91]. Similar effects were observed with 𝛽-D-
er
manopyranose units that showed relevant bands with MD like 3330, 2929, and 2852 depicting
OH stretching, and asymmetric and symmetric lipid CH2 stretch vibration respectively [92].
pe
4. Conclusions

To unleash health beneficiary properties of diosgenin could propose an ameliorate way to cure
and prevent deleterious bodily disorders. Encapsulation with protein and polysaccharide wall
materials was achieved by spray drying which can mask the bitter taste and astringent flavor
ot

of diosgenin. This study revealed about the various spray dried diosgenin powder properties
that predicted 0.3 % diosgenin feed mixture revealed high shelf life imparted by less moisture
tn

content followed by high solubility, and better encapsulation efficiency as compared with other
feed compositions. The presence of different functional groups revealed ranged at1650-1600;
1350-1300; and 1150-1085 containing C=C, S=O, and C-O bonds, and good thermal stability
rin

predicted the good immix held between diosgenin and MD and WPC. Diosgenin's attractive
health promising properties must open a gateway for better development of food,
pharmaceutical, and nutraceutical products.
ep

Acknowledgment
P. Arya thanks Dr. Sunil Khatkar GADVASU Ludhiana for logistic support in conducting the
experiments.
Pr

Conflict of interest

The contributing authors did not have any conflict of interest while preparing the manuscript

This preprint research paper has not been peer reviewed. Electronic copy available at: https://ssrn.com/abstract=4333501
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