DESC:FORM 2

THE PATENTS ACT, 1970
(39 of 1970)
&
THE PATENTS RULES, 2003

COMPLETE SPECIFICATION
[See section 10, Rule 13]

“A process for preparing polymeric encapsulated spirulina powder and a formulation thereof”

PRODYUT BIOTECH INDIA PRIVATE LIMITED, A COMPANY REGISTERED
UNDER THE LAWS OF INDIA, WHOSE ADDRESS IS
FLAT-24E, VENUS APARTMENT, DR. R G THADANI, WORLI SEA-FACE, MUMBAI - 400018, MAHARASHTRA INDIA

THE FOLLOWING SPECIFICATION PARTICULARLY DESCRIBES THE INVENTION AND THE MANER IN WHICH IT IS TO BE PERFORMED

FIELD OF THE INVENTION
The present invention relates to a process for preparing polymer encapsulated spirulina powder. The invention relates to a method for preparing a formulation comprising the polymer encapsulated spirulina powder and a formulation thereof.
BACKGROUND
Microalgae are microscopic organisms found both in seawater and freshwater. Microalgae are rich in dietary fiber such as beta-glucan, vitamins, minerals, polyunsaturated fatty acids such as omega-3 fatty acid and some species have significant amounts of protein of higher quality than plant sources like beans and grains. They have the potential to meet the population’s need for sustainable food supply, specifically with respect to protein demand. Earlier, algae ingredients were mostly used as dietary supplements in different forms, such as powder, capsules, and tablets due to their rich composition in health beneficial compounds (e.g., carotenoids, astaxanthin, omega-3, and docosahexaenoic acid).
The algal extract dietary supplements, nutraceutical compositions, food additives containing algae are known and among different types of algae, the chlorella and spirulina are the most popular due to its high protein content, nutrients, and antioxidants. Recently, the trend is to use the algal ingredients in form of food formulations or beverages. It is known that spirulina is added into drinks such as smoothies, shake, juices, lattes, and lemonades etc. It is known that spirulina has a strong algae or fishy flavor and unpleasant green appearance that does not suit everyone’s palate. The algae containing beverages are known in market but are not popular due to the unpleasant green appearance, fishy smell and grassy taste that makes the drink less attractive to the consumers.
IN202021038970 discloses solid algal composition and brittle containing the solid algal composition. The algal biomass was encapsulated with psyllium husk followed by coating with polymer such as MCC, HPMC or PEG and other additives, colors, flavors etc. The product was converted in the form of beadlets, pellets, granules, and noodles. These beadlets, pellets can be added as inserts or toppings into confectionery, brittle, sandwiches, and other food items.
IN201921007977 discloses dry rewettable spread composition comprising algal biomass, psyllium husk and other additives, flavors. The composition was prepared by freeze drying process to get powdered flakes. The dry rewettable spread composition can be added to liquids such as water, fruit juices, curd, buttermilk, coconut water etc. to form a spread. The spread can be used as bread spread, pizza spread, jam etc.
EP3930748A1 discloses nutraceutical composition comprising spirulina, prebiotic, probiotics and/or synbiotics, cereal, micronutrients. The spirulina along with probiotic, prebiotic is encapsulated using a lipid carrier emulsion. Generally, it is known that the lipid carrier emulsion may have lesser stability and may easily get degraded by the factors such as pH, temperature etc.
The encapsulated spirulina products known in the art discussed above are not suitable to be used in liquid beverages as the encapsulation does not mask the flavor and odour of the algae in beverages. So, there is a need for an efficient encapsulation technique having higher stability, that can retain the bioactivity of the active ingredient and at the same time masks the flavor and odour of the algae.
CN111227257 discloses an industrial process of refining spirulina protein peptide and microencapsulating the spirulina protein peptide in maltodextrin, algin and arabic gum. The process uses spirulina protein peptide instead of using the whole spirulina. The process involves refining of spirulina protein peptide, which is further encapsulated in maltodextrin, algin and arabic gum to obtain microcapsule embedded powder. It may be noted that refined spirulina protein peptide may be devoid of antioxidants, phycocyanin, sodium, potassium, carbohydrates, vitamins, minerals, fats, fibre etc. that are generally present in the whole spirulina biomass. Further, this industrial process to extract the spirulina protein peptide is very tedious and costly procedure.

CN1247089 discloses beverage containing spirulina, wherein the spirulina is dissolved in purified water to form an aqueous solution. It may be noted the whole spirulina biomass does not generally dissolve in water. This prior art discloses that spirulina dissolved in purified water was further complexed with cyclodextrin to get the clad material using microcapsule technology. Further, many Chinese crude drugs like Ganoderma, Rhizoma Polygonati Odorati etc. along with flavouring agents are mixed with the spirulina and processed to get the final granular product. The microcapsule technology using cyclodextrin to encapsulate the spirulina is a highly expensive process. Moreover, it is not mentioned whether the final granular product dissolves in liquid completely and also masks the taste of the Spirulina and other Chinese drugs present therein.
US20090142431A1 discloses to a dietary supplement composition comprising dried biomass of bluegreen algae (Spirulina platensis) along with other additives such as astaxanthin. The manufacturing method includes supercritical carbon dioxide extraction process to extract the astaxantin from the dry biomass of Haemaoccus pluvialis to prepare beadlets and mixing them with dried biomass of spirulina to obtain the said composition. The supercritical fluid extraction technique is a highly energy demanding and expensive process. This prior art is directed to a dietary supplement composition, however, it does not specifically mention whether the composition dispersed in beverages completely masks the taste or flavour of astaxanthin and spirulina content present therein.

Based on the above limitations to the existing technologies, there is an unmet need for providing a formulation containing the nutritional properties of algae, but at the same time the fishy taste or unpleasant smell of algae being masked and which could be easily mixed with liquids and consumed by people of all ages as a health drink, accordingly there is also a need to provide a method for preparing such formulation.

SUMMARY OF THE INVENTION
In an aspect, the present invention provides a process for preparing polymer encapsulated spirulina powder that retain the nutritional properties but at the same time can mask the fishy taste or unpleasant smell of spirulina, such polymer encapsulated spirulina powder being easily converted into a formulation for adding into liquid and consumed by people.
In one aspect, the present invention provides a process for preparing polymer encapsulated spirulina powder, the process comprising forming a polymer solution by adding 15-25 % of a polymer in water, heating the polymer solution at a temperature of 75 oC-90oC or till the solution becomes transparent, cooling the polymer solution to room temperature, adding 5-15% of spirulina powder to the cooled polymer solution and homogenizing the polymer solution and encapsulating the spirulina in the said polymer by spray drying the homogenised polymer solution.
In another aspect the present invention provides a method of preparing a polymer encapsulated spirulina formulation comprising providing a polymer encapsulated spirulina powder, mixing the 20 to 65% of polymer encapsulated spirulina powder with 0.1 to 0.2% of a suspending agent and 0.1 to 0.2% of an anticaking agent.
The method can further comprise of mixing the polymer encapsulated spirulina formulation with a flavouring agent, a sweetener, or combination thereof.
In one more aspect, the present invention provides a formulation comprising 20% to 65% of polymer encapsulated spirulina powder, 0.1 to 0.2% of suspending agent, 0.1 to 0.2% of anticaking agent. The formulation can further comprise a flavouring agent, a sweetener, or combination thereof. The formulation being suitable for converting into a drinkable formulation by adding the polymer encapsulated spirulina to hot or cold milk liquid. The polymer encapsulated spirulina powder can have a particle size of about 100 to 150 microns.
BRIEF DESCRIPTION OF DRAWINGS
Reference will be made to embodiments of the invention, examples of which may be illustrated in the accompanying figures. These figures are intended to be illustrative, not limiting. Although the invention is generally described in the context of these embodiments, it is understood that it is not intended to limit the scope of the invention to these particular embodiments:
The Figure 1 illustrates the microscopic image of the homogenized HICAP 100 solution with spirulina before the spray drying process.
The Figure 2 illustrates the microscopic image of the spirulina algae particles under 4X magnification.
The Figure 3 illustrates the microscopic image of the final polymer encapsulated spirulina powder having a particle size between 100 to 150 microns.
The Figure 4 illustrates the release pattern of phycocyanin from various spirulina products.
The Figure 5 illustrates differential scanning calorimetry thermogram of the spirulina.
The Figure 6 illustrates differential scanning calorimetry thermogram of the polymer encapsulated spirulina powder provided in accordance with an exemplary embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to providing a process for preparing polymer encapsulated spirulina powder that can retain the nutritional properties but at the same time can mask the fishy taste or unpleasant smell of spirulina, such polymer encapsulated spirulina powder being suitable for easily converted into a formulation for adding into liquid and consumed by people.
In an embodiment the present invention provides a process for preparing polymer encapsulated spirulina powder.
In one embodiment, the present invention provides a process for preparing polymer encapsulated spirulina powder comprising:
a) forming a polymer solution by adding 15-25 % of a polymer in water;
b) heating the polymer solution at a temperature of 75 oC-90oC or till the solution becomes transparent;
c) cooling the polymer solution to a room temperature;
d) adding 5-15% of spirulina powder to the cooled polymer solution and homogenizing the polymer solution; and
e) encapsulating the spirulina in the said polymer by spray drying the homogenised polymer solution.
In accordance with the process of the present invention for forming a polymer solution 15-25% of a polymer is added in water. The polymer solution can then be heated to a temperature of 75oC-90oC under stirring or till the solution becomes transparent. Preferably, the polymer solution can be heated to a temperature of 90 °C. Then, polymer solution can be cooled to room temperature before adding about 5-15 % of the spirulina powder. The polymer solution and spirulina powder can then be homogenized for 15-20 minutes. The homogenized polymer solution can be spray dried at an inlet temperature in a range of 150-180 oC and an outlet temperature in a range of 50-80oC, encapsulating the spirulina powder in the polymer. Preferably, the spray drying can be carried out at inlet temperature of 170 oC and an outlet temperature of 63 oC.
In an embodiment, the process further comprises a step of reducing the temperature after the spray drying and collecting the polymer encapsulated spirulina powder. In an embodiment, the temperature can be reduced to 60oC - 70oC after the spray drying process. Preferably, the temperature can be reduced to 70 °C.
In an embodiment 20-23% of the polymer is added in water to provide a polymer solution. In one embodiment, 9-10% of the spirulina powder is added to the polymer solution. Preferably, 9% of spirulina powder can be added to the polymer solution having 21% of polymer dispersed in water.
In an embodiment, the ratio of polymer solution and the spirulina powder can be in a range of 80:20 to 50:50. In another embodiment, the polymer solution and the spirulina powder can be in a ratio of 80:20 to 60:40. In another embodiment, the polymer solution and the spirulina powder can be in a ratio of 70:30.
In an embodiment, the polymer can be selected from the group of food grade modified starch, carbohydrate polymers, starch derivatives, cellulose derivatives, plant exudates, plant extracts, marine, microbial polysaccharides, plant proteins, milk proteins, whey proteins, fats, fatty acids, alcohols, glycerides, waxes, phospholipids. In an embodiments, polymers can be sodium alginate, xanthan gum, acacia, chitosan. In a preferred embodiment, the polymer can be food grade modified corn starch.
In an embodiment, the pH of the polymer solution containing the polymer and water can be in range of 4.0-4.02. In another embodiment, the pH of the spirulina algae added to the polymer solution can be 5.28. In an embodiment, the pH of the homogenized polymer solution before the spray drying can be in the range of 4.17-4.85.
In one embodiment, the polymer encapsulated spirulina powder has a particle size of about 100 to 150 microns.
In an embodiment, the present invention provides a method of preparing a polymer encapsulated spirulina formulation comprising:
i) providing polymer encapsulated spirulina powder prepared by the process in accordance with the present invention;
ii) mixing the 20 to 65% of polymeric encapsulated spirulina powder with 0.1 to 0.2% suspending agent and 0.1 to 0.2% of anticaking agent.
In one embodiment, the suspending agent can be in the range of 0.1 to 0.2%.
The suspending agent can be selected from xanthan gum, gellan gum, guar gum, sodium alginate, acacia gum, other natural, synthetic, or semisynthetic agents.
In one embodiment the anticaking agent can be in the range of 0.1 to 0.2%.
The anti-caking agent can be selected from synthetic substances such as carboxymethyl cellulose, silicon dioxide, sodium dioxide, magnesium carbonate, magnesium stearate and aluminium silicate, magnesium silicate and corn starch.
Without bound by any theory, the suspending agent was found to reduce the sedimentation of the particles when the formulation is added to a liquid. Similarly, the presence of anticaking agents in the formulations was found to prevent the agglomeration during mixing process as well as during storage.
To improve organoleptic properties of the formulation various food grade sweetening agents and flavouring agents can be incorporated in the formulation.
In another embodiment, the method can further or optionally comprise of mixing the polymer encapsulated spirulina powder during the method with a flavoring agent, a sweetener or combination thereof; or alternately, the polymer encapsulated formulation can be mixed with a flavoring agent, a sweetener or combination thereof. The flavoring agent can be selected from kesar, vanilla, cardamon, chocolate, coconut, rose, strawberry, raspberry, blackberry, apricot, apple, blueberry, cherry, mango, black pepper, cardamom, clove, turmeric, red chilli, basil, onion, mint, coriander, tomato, garlic, oregano, other natural, synthetic, or semisynthetic agents. The sweetener can be selected from fructose powder, sucrose, dextrose, or stevia, levulose, lactose, maltose, and other artificial sugar substitutes. The mixing of these flavoring agents, sweeteners with the polymer encapsulated spirulina formulation can be carried out at extreme dry conditions to avoid the moisture, which can protect the spirulina from being spoiled and maintains the integrity of the formulation in storage.
In an embodiment, the present invention discloses a formulation comprising polymer encapsulated spirulina powder, suspending agent and anticaking agent. The polymer encapsulated spirulina powder can be in the range of 20 to 65%. The polymer encapsulated spirulina powder can have a particle size between 100 to 150 microns. The suspending agent can be in the range of 0.1 to 0.2%. The anticaking agent can be in the range of 0.1 to 0.2%.
The suspending agent can be selected from xanthan gum, gellan gum, guar gum, sodium alginate, acacia gum, other natural, synthetic, or semisynthetic agents.
The anti-caking agent can be selected from synthetic substances such as carboxymethyl cellulose, silicon dioxide, sodium dioxide, magnesium carbonate, magnesium stearate and aluminium silicate, magnesium silicate and corn starch.
In another embodiment, the formulation further comprises a flavoring agent, a sweetener or combination thereof. The flavoring agent can be selected from kesar, vanilla, cardamon, chocolate, coconut, rose, strawberry, raspberry, blackberry, apricot, apple, blueberry, cherry, mango, black pepper, cardamom, clove, turmeric, red chilli, basil, onion, mint, coriander, tomato, garlic, oregano, other natural, synthetic, or semisynthetic agents. The sweetener can be selected from fructose powder, sucrose, dextrose, or stevia, levulose, lactose, maltose, other artificial sugar substitutes. The sweetener agent can be 20 to 70%.
In an embodiment, the formulation is suitable for adding to a liquid for providing a drinkable formulation.
In an embodiment, the comprising the polymer encapsulated spirulina powder can be mixed with a liquid. The liquid can be selected from water, milk, juice etc. . The formulation can be added to a cold or a hot liquid. In an embodiment, the hot liquid can have a temperature of about 45 oC.
Examples
Example 1: Preparation of polymer encapsulated Spirulina powder
Figure 2 illustrates the microscopic image of the spirulina algae particles under 4X magnification.

In 700 mL of RO (Reverse osmosis) water, 210 g of HICAP 100 (food grade modified caron starch) was dispersed under stirring. The dispersion was heated slowly to 90 °C under stirring till the solution becomes slightly yellowish to transparent. Further, the solution was allowed to cool till it reached the temperature at 45 °C. Subsequently, Spirulina powder was dispersed in the HICAP 100 solution and homogenized for 15-20 min. The quantities of the sample preparation are illustrated in Table 1.

Table 1: Quantities for polymer encapsulated spray dried Spirulina powder
Sr. No
Ingredients Quantity
1 Water 700gm
2 HICAP 100 210gm
3 Spirulina Powder 90gm

The resulting dispersion of Spirulina was further processed using spray drying procedure. The parameters for the spray drying technique are illustrated in Table 2. The inlet temperature of the spray dryer was set to 170°C. The prepared solution was stirred well and allowed to feed on ASP/ Vacuum (30 HZ) at the rate of 3 mL/min and the outlet temperature was set to 63°C. After the completion of spray drying process, the temperature was brought down to 70 °C and the dried encapsulated material was discharged and collected in a filter bag.

Table 2: Specifications for spray drying process
Sr. No. Parameters Specifications
1. Solution Aqueous
2. Appearance of solution Dark Green
3. pH of Solution (Before drying) 4.17- 4.85
4. pH of RO water and HICAP100 4.0 - 4.02
5. pH of Spirulina Algae 5.28
6. Inlet Temperature 170 °C
7. Outlet Temperature 63°C
8. ASP/Vacuum 30 HZ
9. Automization 1.5 kg
10. Feed Rate 3 mL/min
11. Filter Bag 5 mm
12. Heater 3 KV
13. Nozzle Size 0.7 mm

The polymer encapsulated spirulina powder was found to be homogenous. Figure 3 illustrates the microscopic image of the final polymer encapsulated spirulina powder having a particle size between 100 to 150 microns.
Example 2: Release study of spirulina (Phycocyanin release)
The Phycocyanin release from the spray dried HICAP 100 encapsulated spirulina of Example 1 in comparison with raw spirulina powder, and a known spirulina psyllium beads were studies by dissolution testing method. The release study of phycocyanin from spray dried HICAP 100 encapsulated spirulina, raw spirulina powder, and spirulina psyllium beads was performed in water at room temperature. Samples equivalent to 100 mg of spirulina were taken into muslin cloth and tied to the terminal of the paddle attached with dissolution test apparatus (Model: DS-8000, Lab India, Mumbai). Each sample were placed in a flask containing 500 mL of the dissolution medium (water) at room temperature. Paddles were operated at 50 rpm. At each time interval of 10, 20, 30, 40, 50 and 60 min, 5 mL samples were withdrawn and replaced with fresh medium. The absorbance of the samples was measured by UV-Visible spectrophotometer (Model: UV-1800; Shimadzu India) at 616 nm against the blank. The concentration of phycocyanin was calculated by using slope from standard plot. Percentage of release versus time were plotted to understand the release pattern with respect to time.

Results:
The results of the release pattern of phycocyanin from various products are shown in Figure 4. The graph clearly indicates that phycocyanin release from the spirulina was much faster (91.39±2.81 in 10 min), whereas as compared to spirulina powder the phycocyanin release from the spray dried HICAP 100 encapsulated spirulina (86.65±1.94 in 30 min) in accordance with the present invention as per Example 1 was slower and suitable for drinkable preparations, wherein the phycocyanin release was much slowed from the spirulina psyllium beads (26.62 ± 2.84 in 60 min) not suitable for drinkable preparations.

Example 3: Thermal Analysis by Differential Scanning Calorimetry (DSC):
DSC studies were conducted for spirulina powder (Sample 1), HICAP 100 encapsulated spirulina powder of Example 1(Sample 2), by using DSC instrument (Hitachi DSC-7020) in order to determine the heat stability. The instrument calibration was done with Indium as a standard. About, 2 mg samples were weighed and placed in a closed, hermetic sample pans with pin hole. Samples were heated at a constant rate 10ºC/min and thermograms were obtained. A dry purge of nitrogen gas (50 mL/min) was used for all runs. Samples heat range was set from 30°C to 300oC. Thermal behaviour of the samples was investigated with respect to heat resistance. Thermograms are shown in Figure 5 and 6.
As seen in Figure 5 and Figure 6 thermograms of sample 1 and sample 2 showed broad endothermic peaks at 90C and, 94.1oC respectively. Broad peaks indicated that heat absorption in all three samples is slower. But these values indicated that HICAP 100 encapsulated spirulina (Sample 2) is more heat resistant than spirulina (Sample 1).

From these results, it one can infer that HICAP 100 encapsulated spirulina (Sample 2) can be mixed with cold as well as hot beverages without losing the potency of the spirulina contents. Thus, the heat sensitive natural compositions of spirulina such as proteins, vitamins, minerals, pigments, anti-oxidants and other delicate contents can be protected in accordance with the present invention.
Example 4: Volunteer Assessment of polymer encapsulated spirulina powder
Volunteer study was conducted to assess the taste and flavour of encapsulated spirulina powder as per Example 1 and raw spirulina powder. The results are provided herein the Table 3.
Table 3: Volunteer Assessment of polymer encapsulated spirulina powder
Spirulina Volunteer No. Taste Odour Overall Scoring
Raw Spirulina Powder 1 + + Bad taste and fishy odour
2 + + Bad taste and fishy odour
3 + + Bad taste and fishy odour
4 + + Bad taste and fishy odour
5 + + Bad taste and fishy odour
Encapsulated Spirulina Powder of the present invention 1 ++ ++ No bad taste and no odour
2 +++ ++ No bad taste and no odour
3 +++ +++ No bad taste and no odour
4 +++ +++ No bad taste and no odour
5 ++ ++ No bad taste and no odour
+++: Very good ++: Good +:Poor
The volunteer studies show that the encapsulated polymeric spirulina powder of the present invention was able to mask the taste and odour of spirulina thereby making it suitable for consumption.
Example 5: Content analysis
A. Content analysis of spray dried HICAP 100 encapsulated spirulina of Example 1 (30% spirulina) was performed as per the standard test procedures (Equinox Labs Pvt. Ltd. Mumbai).
B. Content analysis of spray dried HICAP 100 encapsulated spirulina of Example 1 (30% spirulina) was performed as per the standard test procedures (Equinox Labs Pvt. Ltd. Mumbai) for freshly prepared samples (0 month) and sample stored for 3 months at ambient conditions.
Results:
The content analysis results of the HICAP 100 encapsulated spirulina are shown in Table 4. In case of spray dried HICAP 100 spirulina powder, there was no significant variations in protein, carbohydrate, total fat, PUFA and MUFA were observed between 0 month and 3 months storage period. Especially, there was no significant change in the amount of protein were observed. These results revealed that there is no adverse impact of production conditions as well as storage conditions on developed product.
Table 4: Content analysis of the HICAP 100 encapsulated spirulina
Parameters per 100g of product HICAP 100 spirulina*
0 Month 3 Months
Protein 24.09 21.14
Carbohydrate 66.31 69.88
Total Fat 2.20 1.88
PUFA 0.62 0.288
MUFA 0.74 0.652
*Total spirulina content is 30%.
Example 6: Assessment of taste / odor masking of the polymer encapsulated spirulina powder:
A batch of the polymer encapsulated spirulina powder provided as per Example 1 was directly mixed with various fruit juices and evaluated for taste/odor. Initially, about 3.33 g (equivalent to 1 g of spirulina) of HICAP 100 encapsulated spirulina was slowly mixed with 250 mL of various fruit juices in order to facilitate proper hydration to avoid clumping and later vigorously mixed so as to make a uniform dispersion. The level of taste/ odor improvement and sedimentation of particle was assessed as shown in below table 5. Similar procedure was adapted for raw spirulina powder.

Table 5: Evaluation of optimized batch mixed with various fruit juices
Sr. No. Fruit juices used Level of Taste/ Odour improvement Sedimentation in 30 min
(Yes/No)
1 Pineapple +++ No
2 Apple +++ No
3 Watermelon +++ No
4 Grape ++ No
5 Pomegranate ++ No
Note: +++: Highly improved; ++: Improved

Above results indicated that, the raw spirulina powder presented poor taste/ odour (fishy flavor) in all cases; whereas the polymer encapsulated spirulina powder provided in accordance with the present invention as per Example 1 successfully was found to mask unpleasant taste as well as odor and can be directly delivered along with fruit juices.

Example 7: Formulation of polymer encapsulated spirulina
In order to administer the polymer encapsulated spirulina powder along with water or milk and to further improve the taste/ odor of the beverage, initial trials were taken. In these trials, about 3.33 g (equivalent to 1 g of spirulina) HICAP100 encapsulated spirulina as per Example 1 was directly dispersed in 250 mL of water as well as milk in a glass container. The main challenge faced during dispersion process was the formation of clumps, which was further disappeared after prolong stirring process. After complete dispersion, when beverage kept stagnant for 15-30 min, spirulina particles were settled at the bottom of the glass container which was redispersed again after stirring. In order to overcome such challenge, further improvements were done with the formulations. The selection of suitable ingredients and their quantities was done based on various trials, and their roles are explained in Table 6 below. Also, the compositions of various formulations are given in below Table 7.

Table 6: Polymer encapsulated Spirulina formulation
Sr. No. Ingredients Roles
1 Spirulina Active Ingredient
2 HICAP 100 Polymer for encapsulation
3 Crystal fructose powder Natural Sweetener (Low glycemic index)
4 Stevia Natural Sweetener (Zero glycemic index)
5 Sucrose Natural Sweetener (High glycemic index)
6 Xanthan Gum Suspending Agent
7 Guar Gum Suspending Agent
8 Gellan Gum Suspending Agent
9 OL-924-111-1 Masking flavor
10 SWP-007 Masking flavor
11 Cardamom (Liquid) Flavor
12 Raspberry Flavor
13 Blueberry Flavor
14 Vanilla Flavor
15 Chocolate (Brown - Powdered) Flavor
16 Chocolate (White - Powdered) Flavor
17 Cardamom (Powdered) Flavor
18 Pineapple Flavor
19 Carboxy methyl cellulose Anticaking agent
20 Silicon dioxide Anticaking agent
21 Tricalcium phosphate Anticaking agent

Table 7: Composition of various formulations and their evaluation (Quantities calculated for 5.34 g to 7. 34 g of total weight standardized for 30% of HICAP encapsulated spirulina powder)
Formulation Code HICAP 100 Encapsulated Spirulina
(Optimized Batch) (g) Xanthan Gum (g) Guar Gum (g) Gellan Gum (g) Carboxy Methyl Cellulose (g) Silicon Dioxide
(g) Tricalcium Phosphate
(g) Stevia
(g) Crystal Fructose Powder
(g) Sucrose
(g) Flavouring Agent Total Weight
(g)
F1 3.33 0.010 - - 0.010 - - 2 - - Q.S 5.34
F2 3.33 - 0.010 - - 0.010 - - 2 - Q.S 5.34
F3 3.33 - - 0.010 - - 0.010 - - 2 Q.S 5.34
F4 3.33 0.015 - - 0.015 - - 3 - - Q.S 6.345
F5 3.33 - 0.015 - - 0.015 - - 3 - Q.S 6.345
F6 3.33 - - 0.015 - - 0.015 - - 3 Q.S 6.345
F7 3.33 0.020 - - 0.020 - - 4 - - Q.S 7.35
F8 3.33 - 0.020 - - 0.020 - - 4 - Q.S 7.35
F9 3.33 - - 0.020 - - 0.020 - - 4 Q.S 7.35

Optionally in next step, to further improve the taste and flavor, various sweetening agents and flavoring agents (quantity sufficient/as per requirement) were incorporated to ensure the uniform mixing. Moisture should not be allowed during the mixing weighing and mixing process. The resulting formulation was packed and stored in airtight container. As this is dry powder formulation preservative is not included.

Dispersibility and Sedimentation of formulation is provided in Table 8 below:
Table 8: Dispersibility and Sedimentation of formulation
Formulation Code Dispersibility Sedimentation in 30 min.
(Yes/No)
F1 +++ No
F2 +++ No
F3 +++ No
F4 ++ No
F5 ++ No
F6 ++ No
F7 + No
F8 + No
F9 + No
Note: +++: Excellent; ++: Good; +: Poor

Table 9: Composition of various formulations and their evaluation (Quantities calculated for 10 gram of total weight)
HICAP encapsulated spirulina powder (30%) Dispersing agent
[0.1, 0.15 and 0.2%] Anticaking agent
[0.1, 0.15 and 0.2%] Sweetening Agent
Total Weight
(g)
Formulation Code HICAP 100 Encapsulated Spirulina
(Optimized Batch) (g) Xanthan Gum (g) Guar Gum (g) Gellan Gum (g) Carboxy Methyl Cellulose (g) Silicon Dioxide
(g) Tricalcium Phosphate
(g) Stevia
(g) Crystal Fructose Powder
(g) Sucrose
(g) Flavouring Agent
F10 3.33 0.010 - - 0.010 - - 6.65 - - Q.S 10
F11 3.33 - 0.010 - - 0.010 - - 6.65 - Q.S 10
F12 3.33 - - 0.010 - - 0.010 - - 6.65 Q.S 10
F13 3.33 0.015 - - 0.015 - - 6.64 - - Q.S 10
F14 3.33 - 0.015 - - 0.015 - - 6.64 - Q.S 10
F15 3.33 - - 0.015 - - 0.015 - - 6.64 Q.S 10
F16 3.33 0.020 - - 0.020 - - 6.63 - - Q.S 10
F17 3.33 - 0.020 - - 0.020 - - 6.63 - Q.S 10
F18 3.33 - - 0.020 - - 0.020 - - 6.63 Q.S 10
Example 8: Volunteer Assessment of polymer encapsulated spirulina Formulation
Volunteer study was conducted to assess the polymer encapsulated spirulina formulation as per Example 7. The results are provided herein the below Table 10.
Table 10: Assessment of taste and odor
Spirulina Formulation No. Taste Odor Overall Scoring
Raw Spirulina Formulation - + + +
Polymer Encapsulated Spirulina Formulation of the present invention 1 ++ ++ ++
2 ++ ++ ++
3 ++ ++ ++
4 ++ ++ ++
5 ++ ++ ++
6 +++ +++ +++
10 +++ +++ +++
11 +++ +++ +++
12 +++ +++ +++
13 ++ ++ ++
14 ++ ++ ++
15 ++ ++ ++
Note: +++: Excellent, ++:Good; +:Poor
The volunteer studies show that the encapsulated polymeric spirulina formulation of the present invention was able to mask the taste and odour of Spirulina thereby making it desirable for consumption. Additional incorporation of sweetening and flavoring agents further improved the taste and flavor of the formulations.
The embodiments were chosen and described to best explain the principles of the present invention and its practical application, to thereby enable others, skilled in the art to best utilize the present invention and various embodiments with various modifications as are suited to the particular use contemplated.
It is understood that various omission and substitutions of equivalents are contemplated as circumstance may suggest or render expedient, but such are intended to cover the application or implementation without departing from the spirit or scope of the present invention.
,CLAIMS:
We Claim:
1. A process for preparing polymeric encapsulated spirulina powder comprising:
a) forming a polymer solution by adding 15-25 % of a polymer in water;
b) heating the polymer solution at a temperature of 75 oC-90oC or till the solution becomes transparent;
c) cooling the polymer solution to a room temperature;
d) adding 5-15% of spirulina powder to the cooled polymer solution and homogenizing the polymer solution; and
e) encapsulating the spirulina in the said polymer by spray drying the homogenised polymer solution.
2. The process as claimed in 1, wherein in step a), 20-23 % polymer is added.
3. The process as claimed in claim 1, wherein in step d) 9 to 10% of spirulina powder is added.

4. The process as claimed in claim 1, wherein the ratio of polymer solution and the spirulina powder is in a range of 80:20 to 60:40.

5. The process as claimed in claim 4, wherein the ratio of the polymer solution and the spirulina powder is 70:30.

6. The process as claimed in claim 1, wherein the polymer is selected from the group of food grade modified starch, carbohydrate polymers, starch derivatives, cellulose derivatives, plant exudates, plant extracts, marine, microbial polysaccharides, plant proteins, milk proteins, whey proteins, fats, fatty acids, alcohols, glycerides, waxes, phospholipids.

7. The process as claimed in claims 1 to 6, wherein the polymer is food grade modified corn starch.

8. A method of preparing a polymer encapsulated spirulina formulation comprising:
i) providing a polymer encapsulated spirulina powder prepared by the process as claimed in claims 1-7;
ii) mixing the 20 to 65% of the polymeric encapsulated spirulina powder with 0.1 to 0.2% of a suspending agent and 0.1 to 0.2% of an anticaking agent.

9. The method as claimed in claim 8, wherein the suspending agent is selected from xanthan gum, gellan gum, guar gum, sodium alginate, acacia gum.

10. The method as claimed in claim 8, wherein the anticaking agent is selected from carboxy methyl cellulose, silicon dioxide, sodium dioxide, magnesium carbonate, magnesium stearate and aluminium silicate magnesium silicate and corn starch.

11. The method as claimed in claim 8, wherein the method in step (ii) further comprises mixing the polymer encapsulated spirulina formulation with a flavouring agent, a 20 to 70% of sweetener, or combination thereof.

12. The method as claimed in claim 11, wherein the flavouring agent is selected from kesar, vanilla, cardamon, chocolate, coconut, rose, strawberry, raspberry, blackberry, apricot, apple, blueberry, cherry, mango, black pepper, cardamom, clove, turmeric, red chilli, basil, onion, mint, coriander, tomato, garlic, oregano.

13. The method as claimed in claim 11, wherein the sweetener is selected from fructose powder, sucrose, dextrose or stevia, levulose, lactose, maltose.

14. A formulation comprising:
20% to 65% of polymer encapsulated spirulina powder prepared by process as claimed in claim 1 to 7;
0.1% to 0.2%% of suspending agent; and
0.1 to 0.2% of anticaking agent.

15. The formulation as claimed in claim 14, wherein the polymer encapsulated spirulina powder has a particle size of about 100 to 150 microns.

16. The method as claimed in claim 14, wherein the suspending agent is selected from xanthan gum, gellan gum, guar gum, sodium alginate, acacia gum.

17. The method as claimed in claim 14, wherein the anticaking agent is selected from carboxy methyl cellulose, silicon dioxide, sodium dioxide, magnesium carbonate, magnesium stearate and aluminium silicate magnesium silicate and corn starch.

18. The formulation as claimed in claim 14, wherein the formulation further comprises a flavouring agent, a 20 to 70 % of sweetener, or combination thereof.

19. The formulation as claimed in claim 18, wherein the flavouring agent is selected from kesar, vanilla, cardamon, chocolate, coconut, rose, strawberry, raspberry, blackberry, apricot, apple, blueberry, cherry, mango, black pepper, cardamom, clove, turmeric, red chilli, basil, onion, mint, coriander, tomato, garlic, oregano.

20. The formulation as claimed in claim 18, wherein the sweetener is selected from fructose powder, sucrose, dextrose or stevia, levulose, lactose, maltose.

Dated this 12th day of January, 2023

For Prodyut Biotech India Private Limited
By their Agent

(ANSHUL SUNILKUMAR SAURASTRI) (IN/PA 3086)
KRISHNA & SAURASTRI ASSOCIATES LLP