Description:FIELD OF THE INVENTION
The present invention relates to a hard empty capsules and the composition for the same. The composition used here in this invention utilizes the plant based organic material i.e., Sago starch. The present invention also discloses the hard empty capsule composition comprising pullulan along with the plant based organic material i.e., Sago starch.
The present invention further relates to the process of preparing the hard empty capsules and thereby produces the impact resistant, deformation resistant and fast dissolving hard empty capsules.

BACKGROUND OF THE INVENTION
A capsule – an oral dosage form is known since ages wherein the term “capsule” is derived from the Latin word – “Capsula” which means “a small container.”
Capsules are solid dosage form wherein a medicinally active ingredient is enclosed within the hard or soft gelatin capsule shell. Most of the times, an oral dosage in the form of hard shell capsules are used for the delivery of life-saving drugs, mineral, vitamins or other nutritious ingredients. Hard shell capsules enable reliable dosing, portability and high consumer compliance.
The capsule shell is an egg-shaped hollow shell. The capsule shell has ease of swallowability, excellent taste masking, good bioavailability, and can be dissolved rapidly, reliably and safely. One type of commonly used capsule is a two-piece hard shell capsule, typically made from edible pharma or food grade polymers such as gelatin, modified starch, or modified cellulose derivatives along with additives, processing aids, auxiliary materials and is used for containing solid powder, particles, liquid or semi solids. In most cases, capsule shell manufacturing starts with the preparation of mucilage. In the next step, plurality of moulding pins made of special grade of stainless steel are dipped into the mucilage for a certain amount of time and certain depth, separately for capsule cap and body part. This process is called dipping and lasts just for a short period of time before the pins get removed from the mucilage and are transferred towards the drying area while spinning around their axis in order to get the mucilage distributed evenly. In the drying area, pins pass several drying stages so the mucilage gets converted in thin rigid film and achieves desired moisture content. After drying, capsule body and cap halves are stripped off the pins, cut to a correct length and in the final step joined together into a pre-lock position before they get ejected into containers for transport and filling.
The existing capsules are generally used by combining a capsule cap and a capsule body wherein longer body has an outside diameter, and a relatively shorter cap has an inside diameter that will just fit over each other. Capsule cap and body being two independent parts, cap fits snugly over the body,
There lie many advantages with the capsule dosage forms such as their attractive appearance, encapsulation of drugs with unpleasant taste and odour, easy administration, readily solubilization of gelatin or other polymer at gastric pH and thus capsule dosage forms has high consumer acceptance.
Owing to this high consumer acceptance, various methods and techniques are developed over the years to prepare capsule shells. Hard capsule shells are already present in market however the composition used for their preparation is either an animal origin such as gelatin or in synthetic or semi synthetic form such as Hydroxy propyl methyl cellulose or hydroxypropyl starch.
Furthermore, starch based capsules has also been worked upon but in the form of soft starch capsule. There has always been a challenge in overcoming the high viscous solutions of starches at a very low concentration in water, which is a bottleneck for getting capsules of appropriate strength and weight. Other disadvantages of these starch capsules are slow dissolution of the inside content of the capsules. Also, due to lower molecular weight they depict shell cracking and/or shattering.
United States Patent Publication No. 6,375,981 discloses a soft gel capsule that comprises a sealed capsule wall wherein the capsule wall comprises starch-based composition prepared with water. The modified starches suitable for use in this reference are thermally converted, fluidity or thin boiling type products derived from chemically modified starches. Thus, the hydrolyzed starch that is used in this art is boiled under conditions and thus it leads to a complete destruction of the starch grains. As we know, the long starch macromolecules have positive influence on the mechanical properties, this art faces the inferior mechanical properties of the soft capsules due to the destruction of the starch grains.
Chinese Patent Publication No. CN 1333006 discloses the vegetable capsule of starch composition and its preparation process. The composition discloses in this reference include 10 parts starch, 1-6 parts plasticizer, 0.15-2 parts gel agent, proper amount of surface-active agent, and other auxiliary ingredients.
European Patent Publication No. EP 1103254 discloses method for producing a starch-containing shaped body, a homogenized starch-containing mass, and an extrusion method for manufacturing a soft capsule. Owing to the requirements of extruders, the manufacturing process is complex wherein the process is also defined using welding step at high temperature to form a one-piece capsule shell.
Being the non-animal, organic material - starch obtained from plant sources is also used for preparation of soft capsules. Starch is a much less expensive raw material than gelatin. However, casting methods for producing soft starch capsules from aqueous starch solutions are limited due to the necessity of using a low starch content and a high-water content for such solutions. Mixtures of destructured or dissolved starch typically become so viscous at a starch content of 5% that simple casting methods at least are no longer possible. The reason for this is the extremely high molecular weight of starch, which may be as high as 100,000,000 g/mol.
The starch soft capsules manufactured using the solutions of degraded starch or extruded starch materials possess the greatly contradictory combination of pourability, i.e., low viscosity and essentially destroyed starch particles. Consequently, soft capsules produced according to the above United States Patent Publication No. 6,375,981 and European Patent Publication No. EP 1103254 essentially contain only starch of destructuring stage.
In the past, the injection moulding of two-part starch capsule has also been known from United States Patent Publication No. 4,738,818; United States Patent Publication No. 4,738,724; United States Patent Publication No. 4,539,060; and United States Patent Publication No. 4,591,475. The capsules thus obtained using the method, as disclosed in these patent publications, substantially consisted of amorphous starch which led to brittleness and the capsules formed were not resistant to impact and deformation in high performance filling units.
Moreover, soft starch capsules are usually obtained by extrusion, which requires expensive extruders. A homogeneous starch melt of a high viscosity is produced from the starch which is typically present in a granular form at temperatures of more than 100°C. in plasticization under the influence of mechanical energy in the form of shearing and this starch melt is then pressed through a slotted nozzle under high pressures to first produce a starch film. Due to the high mechanical energy input the molecular weight of the starch is greatly reduced, which is a disadvantage for the mechanical properties of the film, and furthermore, the macromolecules become oriented in the longitudinal direction of the film during the flow processes that take place at the nozzle, so the film is anisotropic, which is a disadvantage for further processing. After shaping there is no gelation when starch films are extruded and instead after the shaping the temperature of the film drops so the strength of the film increases somewhat. This film is then processed further to form soft capsule shells.
In light of above stated reasons, many inventors have tried to improve the mechanical strength of the capsules to develop other hard empty capsules consisting of material from plant based origin.
Japanese Patent Publication No. 202003 discloses the capsules made up of mixtures of hemicellulose, carboxymethyl cellulose or native starch, which are polysaccharides of the type of poly(ß-D-glucan) or poly(a-D-glucan), respectively. International Patent Publication No. WO 00/18835 discloses the capsules consisting essentially of starch ethers and oxidized starch are disclosed, whereas International Patent Publication No. WO 96/10996 describes capsules based on I(iota)-carrageenan.
United States Patent Publication No. 5,698,155 and United States Patent Publication No. 5,431,917 describe water soluble cellulose derivatives for the manufacture of hard- shell capsules in a dip moulding process. Because of the expensive raw materials involved these materials are generally not accepted by capsule consumers. Thus, in the art no fully satisfactory hard-shell capsules consisting of non-animal material have been described nor are they are available to the date.
However, despite the so many attempts, none have succeeded in manufacturing hard capsules or other capsules of plant based origin in large quantities with sufficient uniformity to be suitable for filling in modern high-speed filling machines.
Therefore, considering the aforementioned facts, there exists a need to develop new hard empty capsules comprising a material from plant based organic material as an excipient wherein such plant based organic material provides processable viscosity. There further exists a need to prepare the hard empty capsule with high solid content enabling to form capsules of appropriate weight, mechanical strength, and comparatively lesser dissolution time.
The invention here resolves the issues faced by the various prior arts, where viscosities of the starches are very high at low concentration thereby the weight and the strength of the capsules are within the required limit dissolution time of the capsules is not high. The invention as described herein uses no other method such as destructing of starch granules or injection molding which ruptures the crystalline structure of starch.
Thus, it is an object of the present invention to provide hard empty capsules made from non-animal, plant based material, which should be highly resistant to impact and deformation in order to be applicable in state-of-the-art high performance filling equipment, convenient for medicinal purposes, and these capsules should be superposable and tenable for prolonged periods of time.

SUMMARY OF THE INVENTION
The invention discloses the hard empty capsules prepared from plant based organic material i.e., Sago starch as a primary film forming polymer. The capsules prepared according to the invention are most likely to be an impact and deformation resistant and thereby enabling the prepared hard empty capsules applicable to high performance filling equipment, convenient to medical use along with superposable and tenable property for prolonged period.
The invention further discloses the process to prepare the hard empty capsules from plant based organic material i.e., Sago starch as a primary film forming polymer. This material provides a good workable viscosity and faster dissolution when blended with organic pullulan. Other and more detailed objects of this invention will be apparent from the following description drawings and claims.

DETAILED DESCRIPTION OF THE INVENTION
Capsules are solid oral dosage form wherein a medicinally active ingredient is enclosed within the hard or soft polymer capsule shell.
The term “formulation” or “composition” as used throughout the specification refers to the hard empty composition comprising plant based organic material Sago starch in combination with food and/ or pharmaceutically acceptable excipients.
The term “polymer” as used throughout the specification can be selected from the group consisting of cellulose derivatives such as cellulose acetate; cellulose acetate phthalate (CAP), hydroxypropyl methyl cellulose (HPMC); hydroxypropyl methylcellulose acetate succinate (HPMCAS), hydroxypropyl methyl cellulose phthalate (HPMCP), pullulan, any form of native starches, modified starches or any combination thereof.
The term “plasticizer” as used throughout the specification can be selected from the group consisting of polyvinyl alcohols, polyvinyl pyrrolidines (Plasdone), glycerine, sorbitol, propylene glycols, sorbitan solutions, or any combination thereof. The plasticizer(s) used herein help to make the shell elastic and pliable and to minimize brittleness and cracking.
The term “gelling agent with gel promoters” as used throughout the specification can be selected from the group consisting of gellan gum-EDTA&Na2CO3, Agar-KCl/NaCl, Carrageenan-KCl, Locust bean gum-EDTA&Na2CO3 and combinations like Locust bean Gum - Xanthan gum, Guar gum-KCL, Guar gum – KCL+ Carrageenan, Guar gum + LBG-Xanthan gum combination, pectin-EDTA, ,
Acacia Gum-potassium chloride/sodium chloride, Carbomers (carbomer 934P, carbomer 940, and carbomer 941 with KCl, NaCl, K2CO3, Na2CO3) or any combination thereof alone or jointly. Primarily, gelling agents along with gel promoters are used to achieve film forming as well as acid resistant properties.
The term “stabiliser” as used throughout the specification can be selected from glycerine, propylene glycols, sorbitol, sorbitan solutions, silicone di oxides, or any combination thereof. The stabiliser(s) used herein help to prevent or to minimize the capsule shell defects such as sticking, tacking, softening and premature dissolution of the capsule shell. They also minimise oxidation or degradation of the active ingredient fill or shell.
The term “surfactant” as used throughout the specification can be selected from Sodium Lauryl Sulphate, Tween 80, Polyoxyethylene (80) sorbitan monooleate (Essac 80), Sucrose monopalmitate (Habo monoester 90), Glycerol stearates, sugar esters, rice bran oil esters derived from rise husks, Coco glucoside, Decyl glucoside, Lauryl glucoside, Sucrose cocoate, Caprylyl/Capryl glucoside, Succinylated Monoglycerides (SMG), Ethoxylated Monoglycerides (EMG), Propylene-glycol monoesters (PGME), polyglycerol esters (PGE), polysorbates or any combination thereof. The surfactants used herein help to improve film formation on lubricant polished stainless-steel pins. And to prevent or to minimize the defects such as weak area, thin wall, holes in the capsule shell. They may also minimise oxidation or degradation of the certain active ingredient fill or shell.
In one aspect, the invention provides the hard empty capsule prepared from plant based organic material such as Sago starch as a primary film forming polymer.
Sago starch is an organic material obtained from the pith of Palm trees. Sago starch is nothing but a starch or spongy core tissue of tropical palm stems, especially from Metroxylon sagu. Metroxylon sagu, is found in tropical lowland forest and freshwater swamps across Southeast Asia and New Guinea and is the primary source of Sago starch. Several other species of the genus Metroxylon, particularly Metroxylon salomonense and Metroxylon amicarum, are also used as sources of Sago starch. Traditionally, Sago starch is used to treat fiber in a process called sizing, which makes fibers easier to machine.
In this invention, the inventors have used Sago starch from Metroxylon sagu to prepare the hard empty capsules and surprisingly found that the capsules prepared according to this invention are more suitable, as compared to the existing capsules described in background, for further capsule filling process.
In this invention, the inventors have used starch wherein starch contains polymer chains of glucose units with a high degree of regularity, crystalline clusters of double helices which consist of two glucans - amylopectin and amylose. The crystalline structure of Sago starch is related to the gelatinization characteristics wherein Sago starch granules are oval with temple-bell like shape. The mean diameter of Sago starch granules is 37.59 µm and they exhibit a Maltese cross, indicating the presence of some common internal ordering.
In one embodiment, the Sago starch from its X-ray diffraction pattern shows a peak at around 5.6, 17, 18, and 23° (2? for Cu Ka), which corresponds to 1.58, 0.521, 0.492, and 0.386 nm, respectively. Sago starch is classified as a C type (a mixture of A type and B type as an accessary), containing slightly higher content of B type in the basal portion of Sago starch palm trunk. Low viscosity of Sago starch amylopectin is explained by the presence of smaller molecule with a slightly higher number of long chains than the high-viscosity amylopectin. The amylopectin chain distribution of Sago starch is composed of four fractions with the different chain lengths of Fraction I (22.9 ± 0.8%), Intermediate Fraction (3.9 ± 0.4%), Fraction II (17.2 ± 0.4%), and Fraction III (56.0 ± 1.4%).
In one aspect, one unit (a total of 12 glucose residues consisting of 6 glucose residues making a double helix forming 1 unit) of A-type starch, monoclinic structure, holds eight water molecules Meanwhile, one unit of B-type starch, hexagonal structure, holds 36 water molecules in the cavities of the structure. In addition, C-type starch also was proposed to be a mixture of A and B type. However, C type always consists of A and B type.
Starch gelatinization is the disruption of molecular order within the starch granule manifested in irreversible changes in properties such as granular swelling, native crystallite melting, loss of birefringence, and starch solubilization. The gelatinization temperature and enthalpy of Sago starch determined by a differential scanning calorimeter (DSC) are 69.4–70.1°C and 15.1–16.6 J g-1, depending on the moisture content, degree of a crystallinity within the granule, granule size, and the amylose to amylopectin ratio. The observation of granular birefringence (Maltese cross) under polarized light is one of the useful tools to determine the gelatinization behaviour of Sago starch.
In one aspect, the viscosity of the Sago starch defines the invention wherein hard empty capsules, prepared according to the invention, are made up of starch with processable viscosity and high solid content enabling to form capsules of appropriate weight, mechanical strength and comparatively lesser dissolution time.
In one embodiment, the invention provides the hard empty capsule composition comprising plant based organic material – Sago starch, as primary film forming polymer, obtained from the pith of palm trees.
In another embodiment, the invention provides the hard empty capsule composition comprising primary film forming polymer as plant based organic material – Sago starch obtained from the pith of palm trees blended with organic pullulan as secondary film forming polymer. Pullulan is a polysaccharide polymer consisting of maltotriose units, also known as a-1,4- ;a-1,6-glucan'. Three glucose units in maltotriose are connected by an a-1,4 glycosidic bond, whereas consecutive maltotriose units are connected to each other by an a-1,6 glycosidic bond. Pullulan is produced from starch by the fungus Aureobasidium pullulans. Pullulan is an odorless white powder and is easily soluble in water and safe and non-toxic.
In one embodiment, the pullulan of the present invention has preferably an average molecular weight comprised between about 100 KDa and 400 KDa, preferably between 150 KDa and 350 KDa, more preferably between 200 KDa and 330 KDa; and has a melt viscosity at about 60° C. between about 500 cPs and 1500 cPs, preferably between about 800 cPs and 1000 cPs. The pullulan used in this invention is certified organic pullulan from eminent certification authority.
In one aspect of the invention, the hard empty capsule composition comprises plant based organic material – Sago starch obtained from the pith of palm trees blended with organic pullulan as secondary film forming polymer. HPMC and pullulan capsules are regarded as noteworthy alternative to gelatin capsules in terms of their consumer acceptability.
In another aspect, the intrinsic viscosity for amylose from Sago starches are varied between 310 and 460 ml/g while for amylopectin the values are varied between 210 and 250 ml/g. The molecular weight for amylose is found to be in the range of 1.41×106 to 2.23×106 while for amylopectin it varies in the range of 6.70×106 to 9.23×106.
In one embodiment, the invention provides the hard empty capsule composition comprising plant based organic material – Sago starch obtained from the pith of palm trees and blended with the other excipients. The excipients include herein are, but not limited to, polymer, plasticizers, stabilizer, surfactants, gelling agents with gel promoters thereof. All the excipients used herein are added as a percentage of total dry weight of Sago starch and organic pullulan.
In another embodiment, the content of Sago starch present ranges from about 20% to about 80% in the total composition.
In another embodiment, the content of organic pullulan present ranges from about 10% to about 70% in the total composition.
In one aspect of the invention, the gelling agent with gel promoters used in the invention ranges from about 0.2% to about 10% of total dry weight of Sago starch and Organic pullulan.
In another aspect, the plasticizers used in the composition of the invention ranges from about 0.1% to about 8% of total dry weight of Sago starch and Organic pullulan.
In one embodiment, the surfactant used in the composition of the invention ranges from about 0.01% to about 8% of total dry weight of Sago starch and Organic pullulan.
In one embodiment, the invention provides the process to prepare hard empty capsule comprising-
a. Preparing the melter mixer stock solution (mucilage)
b. Preparing the feed tank using melter mixer stock solution (mucilage)
c. Dipping the capsule mould for capsule body and capsule cap in the dip bath
d. Drying and stripping of capsule body and capsule cap from the capsule mould
e. Cutting the stripped shells and joining of the body part and cap part to form empty hard capsule.
In another embodiment, the invention provides the process to prepare the melter mixer stock solution (mucilage) comprising-
a. Blending the plant based organic Sago starch, Pullulan and other additives such as plasticizers, stabilizer, surfactant, and gelling agent with gel promotors along with the purified water to prepare melter mixer stock.
b. Stirring and cooling the stock solution to a pre-defined temperature.
In one aspect of the invention, plant based organic Sago starch, Pullulan and other additives such as gelling agents with gel promoters such as Carrageenan-KCl, Locust bean gum-EDTA&Na2CO3 and combinations like Locust bean Gum - Xanthan gum, Guar gum-KCL, Guar gum – KCL+ Carrageenan, Guar gum + LBG-Xanthan gum combination, pectin-EDTA, ,
Acacia Gum-potassium chloride/sodium chloride, Carbomers (carbomer 934P, carbomer 940, and carbomer 941 with KCl, NaCl, K2CO3, Na2CO3) alone or combination . Plasticisers such as glycerine, polyvinyl alcohol (PVA), carboxymethylcellulose (CMC), polyvinylpyrrolidone (plasdone), sorbitol, Triethyl citrate(TEC), polyethylene glycol (PEG) alone or combination and purified water of 95ºC ±4 ºC are blended together over the time period of 90 to 120 min. The solution, is stirred at a speed of 100 to 200 RPM and the obtained stock solution is cooled to 70ºC ±2 ºC.
In one embodiment, the invention provides the process to prepare the feed tank comprising mixing of melter mixer stock solution along with the other additives, if any. The other additives may include coloring agent (natural and/or synthetic), opacifiers, super disintegrant, surfactant, and/or combination thereof.
In one aspect, the invention provides the process to prepare hard empty capsule comprising-
a. Blending the plant based organic Sago starch, Pullulan and other additives such as gelling agents along with gel promoter Carrageenan-KCl, Locust bean gum-EDTA&Na2CO3 and combinations like Locust bean Gum - Xanthan gum, Guar gum-KCL, Guar gum – KCL+ Carrageenan, Guar gum + LBG-Xanthan gum combination, pectin-EDTA,
Acacia Gum-potassium chloride/sodium chloride, Carbomers (carbomer 934P, carbomer 940, and carbomer 941 with KCl, NaCl, K2CO3, Na2CO3) alone or combination. Plasticisers such as glycerine, polyvinyl alcohol (PVA), carboxymethylcellulose (CMC), polyvinylpyrrolidone (plasdone), sorbitol, polyethylene glycol, Triethyl citrate (TEC) alone or combination along with the purified hot water to prepare melter mixer stock;
b. Stirring and cooling the stock solution;
c. Preparing the feed tank using melter mixer stock solution;
d. Adding necessary additives such as colouring agent (natural and/or synthetic), opacifiers, super disintegrants, surfactants etc alone or combination which are generally accepted and known or used in the capsule manufacturing industry.
e. Dipping the capsule mould for capsule body and capsule cap in the dip bath;
f. Drying and stripping of capsule body shell and capsule cap shell from the capsule moulds;
g. Cutting the stripped shells and joining of the body part and cap part to form empty hard capsule.
In another aspect of the invention, the process to prepare hard empty capsule comprises dipping of the capsule moulds in the stock solution wherein dip bath temperature is maintained at about 65±15°C under constant stirring.
In further aspect, during dipping the process pin bar temperature is maintained at about 20°C to about 30°C.
In another aspect of the invention, the process to prepare hard empty capsule further comprises drying of capsule moulds coated with stock solution. The drying temperature is maintained at temperature between 20 to 35°C with absolute humidity of 6 to 9 gm/kg of dry air. The velocity of air is above 700 FPM. On completion of drying, the capsule cap and capsule body are stripped off from the capsule moulds, cut to appropriate length and are joined together to form hard empty capsule.
The present invention is further explained in detail by referring to the following, which are not to be construed as limitative.
Examples:
Process to prepare films and hard empty capsule for evaluation and conclusion.
A. Preparation of Stock Solution
1. The water bath with temperature at 98±1°C was set and ensured the maintaining of the solution temperature at 95±1°C throughout. DM water of known quantity was later weighed, when the required temperature was achieved.
2. All the additives and film forming polymers were added as per matrix as shown in table 1 below. The quantity for all the additives is percentage of total dry weight of primary and secondary film forming polymers. (Sago starch and pullulan)
3. To the solution of step 1, KCl was added and stirred for 10 min wherein RPM was maintained at 100 to 200 RPM.
4. To the solution of step 3, ESSAC 80 was added and stirred for 10 min.
5. To the solution of step 4, Glycerol was added and stirred for 10 min.
6. To the solution of step 5, PVA was added and stirred for 10 min.
7. To the solution of step 6, Plasdone was added and stirred for 15 min.
8. Later, to the solution of step 7, the mixture of measured quantity of Sago starch & Pullulan was added slowly to avoid lumps formation during addition of material. Here during this step, the RPM was maintained at 100-200 RPM until the addition of powder was finished.
9. After adding the powder in step 8, the stirring speed was increased to 200-300 RPM and was maintained for the next 3 hrs, until complete dispersion of starch material was achieved. During this step, the vessel was covered adequately to ensure minimum evaporation loss.
10. KC(Carrageenan) solution was prepared separately in cold water at 15°C to 16°C by mixing known quantity of powder manually for 15 min and waited until uniform dispersion was achieved.
11. KC solution of step 10, was then transferred to hot water batch kept at 80°C and the stirring was maintained at speed at 100-200 RPM for 30 min to completely dissolve KC in water.
12. The prepared KC solution of step 11 was later added to the Sago starch: Pullulan vessel of step 9 and mixed for 15 to 20 mins.
13. The set temperature of water bath was decreased to 70°C temperature and the stirring RPM was reduced 70-120 RPM. This condition was later maintained for next 30 min to 45 min to clear the bubbles generated during mixing process and homogenization of the solution.
14. After the temperature of solution decreased to 65°C to 70°C; viscosity, solid content, and gel flow of the solution was recorded.
15. Viscosity was measured by Brookfield viscometer, solid content was measured gravimetrically by suitable in house method developed at ACG ACPL. Also, gel flow which is measure of gelling ability of film was measured by inhouse developed equipment at ACG ACPL.

B. Manufacturing and Evaluation of Films for Feasibility
16. The solution as prepared in step 14 above was then poured in film maker developed in house by ACG-ACPL.
17. Films of 100 mm width and 600 mm length were casted precisely having uniform film thickness of 100 microns (dry film thickness).
18. The films were further dried at room temperature air in open condition. After drying they were removed and measured for moisture and film properties such as film formation, stiffness, clarity etc visually.
19. The observations were tabulated in Table 2 below.

C. Preparation of Feed Tank solution and Dipping Pins to Manufacture Capsules
20. Similar steps from step 1 to 14 were followed. However, this time the composition followed was as per Table 3 and Table 5 as given below.
21. Viscosity was measured by Brookfield viscometer; solid content was measured gravimetrically by suitable in-house method developed at ACG ACPL. Also, gel flow which is measure of gelling ability of film was measured on inhouse developed equipment at ACG ACPL.
22. On arriving at the viscosity, solid content and gel flow within the acceptable limit, the melter mixer stock solution as prepared in step 14 was transferred to dip bath.
23. The dip bath temperature and RPM were maintained at 65±5°C and 40 to 60 RPM respectively.
24. The pin bar temperature was maintained at 23°C to 25°C.
25. The machine speed was fixed at 20 bars per min speed.
26. The dipping was carried out by setting a suitable dipping and withdrawal profile.
27. During the process parameters such as pick up weight, solution viscosity, solid content and gel flow were monitored at regular interval to ensure formation of capsule shell of appropriate weight and dimension.

D. Drying, Stripping, Cutting and Joining of Capsule Shell
28. On completion of dipping, the capsule moulds coated with stock solution were transferred for drying.
29. The coated pin bars were then subjected to the stream of air with velocity between 1000 to 1500 FPM having temperature of 20 to 28°C and absolute humidity of 7 to 8 gm/ kg of dry air. The drying time required was below 40 mins.
30. On drying, the capsule body and capsule cap were stripped off from the capsule moulds, cut to appropriate length and joined together to form hard empty capsule.
31. The capsules so formed were evaluated for dimensional parameters as well as for Organic content as defined by USDA prescribed method.
32. Also, they were evaluated for dissolution test as prescribed in USP for immediate release pH (0.1N HCl using paddle and sinker method at 37°C temperature). The % drug release was measured and tabulated at regular interval. The model formulation used was Acetaminophen.
The observations were as tabulated in Table 4 and Table 6 below:
Table 1: Trial Formulations of Sago Starch:Pullulan with excipients PVA, CMC and Plasdone for making films

Table 2: Evaluation of film properties of trials as per table 1

Table 3: Formulations with CMC and additive for manufacturing capsules

Table 3 shows the compositions with CMC plasticizer (Cekol) wherein (30) depicts Cekol 30 grade, (700) depicts Cekol 700 grade and (30000) depicts Cekol 30000 grade
Table 4: Evaluation of capsules with formulations of CMC and their dissolution

Table 5: Formulations with Plasdone (Polyvinylpyrrolidone) Additive for Manufacturing Capsules

Table 6: Evaluation of capsules with formulations of Plasdone (Polyvinylpyrrolidone)

Conclusion:
Thus, from the Table 2 above, it can be inferred that the good films are formed using some of the compositions as disclosed in Table 1.
From the Table 4 above, it can be inferred that with some trial combinations, good dissolution can be achieved with CMC as Plasticizer. All the compositions as disclosed above comply to USDA Organic content criterion with the possibility to get organic certification. The plasticizer used herein is CMC of different molecular weights.
As seen from Table 6 above, in these trials, the plasticizer used is PVP in place of CMC. With PVP as plasticizer in many trial combinations, good dissolution can be achieved. All the compositions comply to USDA Organic content criterion with the possibility to get organic certification.
,
C , Claims:1. The hard empty capsule comprising plant based organic material Sago starch obtained from the pith of palm trees as primary film forming polymer and blended with organic pullulan as secondary film forming polymer.
2. The Sago starch, as claimed in Claim 1, is obtained from tropical palm stems, especially from Metroxylon sagu.
3. The hard empty capsule as claimed in Claim 1, comprising plant based organic material Sago starch obtained from the pith of palm trees and organic pullulan blended with other excipients such as plasticizers, stabilizer, surfactant, and gelling agent with gel promotors.
4. The other excipients, as claimed in Claim 3, are added as a percentage of total dry weight of Sago starch and Organic pullulan.
5. The content of Sago starch obtained from the pith of palm trees present in the dry capsule, as claimed in Claim 3, ranges from about 20% to about 80%.
6. The content of Organic pullulan present in dry capsules, as claimed in Claim 3, ranges from about 10% to about 70%.
7. The gelling agent with gel promotors, as claimed in Claim 3, is selected from the group consisting of Gellan gum-EDTA&Na2CO3, Agar-KCl/NaCl, Carrageenan-KCL, Locust bean gum-EDTA&Na2CO3 and combinations like Locust bean Gum - Xanthan gum, Guar gum-KCL, Guar gum – KCL+ Carrageenan, Guar gum + LBG-Xanthan gum combination, pectin-EDTA, ,
Acacia Gum-potassium chloride/sodium chloride, Carbomers (carbomer 934P, carbomer 940, and carbomer 941 with KCl, NaCl, K2CO3, Na2CO3) and combination thereof.
8. The gelling agent with gel promoters as claimed in Claim 7, ranges from about 0.2% to about 10% of total dry weight of Sago starch and Organic pullulan.
9. The plasticizers, as claimed in Claim 3, is selected from the group consisting of polyvinyl alcohols, polyvinyl pyrrolidines (Plasdone), glycerine, sorbitol, propylene glycols, sorbitan solutions, or any combination thereof.
10. The plasticizers, as claimed in Claim 9, ranges from about 0.1% to about 8% of total dry weight of Sago starch and Organic pullulan.
11. The surfactants, as claimed in Claim 3, is selected from the group consisting of Sodium Lauryl Sulphate, Tween 80, Polyoxyethylene (80) sorbitan monooleate(Essac 80), Sucrose monopalmitate (Habo monoester 90), Glycerol stearates, sugar esters rice bran oil esters derived from rise husks, Coco glucoside, Decyl glucoside, Lauryl glucoside, Sucrose cocoate, Caprylyl/Capryl glucoside, Succinylated Monoglycerides (SMG), Ethoxylated Monoglycerides (EMG), Propylene-glycol monoesters (PGME), polyglycerol esters (PGE), polysorbates or any combination thereof.
12. The surfactants, as claimed in Claim 11, ranges from about 0.01% to about 8% of total dry weight of Sago starch and Organic pullulan.
13. The pullulan, as claimed in Claim 3 is certified organic pullulan from eminent certification authority.
14. The process to prepare hard empty capsule comprising:
a. Preparing the melter mixer stock solution
b. Preparing the feed tank using melter mixer stock solution
c. Dipping the capsule mould for capsule body and capsule cap in the dip bath
d. Drying and stripping of capsule body and capsule cap from the capsule mould
e. Cutting the stripped shells and joining of body part and cap part to form hard empty capsule.
15. The process to prepare the melter mixer stock solution of Claim 14 comprising;
a. Blending the plant based organic Sago starch, Pullulan and other additives such as plasticizers, stabilizer, surfactant, and gelling agent with gel promotors along with the purified hot water to prepare melter mixer stock
b. Stirring for adequate mixing with homogenisation and then cooling the stock solution to pre-defined temperature.
c. optionally adding additives such as natural colouring agent, synthetic colouring agent, opacifiers, surfactants, super disintegrants, alone or combination which are generally accepted and known or used in the capsule manufacturing industry;
d. Dipping the capsule mould for capsule body and capsule cap in the dip bath
e. Drying and stripping of capsule body and capsule cap from the capsule moulds
f. Cutting the stripped shells and joining of the body part and cap part to form hard empty capsule.
16. The process to prepare hard capsule comprising;
a. Blending the plant based organic Sago starch, Pullulan and other additives such as gelling agents (Carrageenan-KCl), Locust bean gum-EDTA&Na2CO3 and combinations like Locust bean Gum - Xanthan gum, Guar gum-KCL, Guar gum – KCL+ Carrageenan, Guar gum + LBG-Xanthan gum combination, pectin-EDTA, , Acacia Gum-potassium chloride/sodium chloride, Carbomers (carbomer 934P, carbomer 940, and carbomer 941 with KCl, NaCl, K2CO3, Na2CO3) alone or combination , Plasticisers such as glycerine, polyvinyl alcohol (PVA), carboxymethylcellulose (CMC), polyvinylpyrrolidone (plasdone), sorbitol, polyethylene glycol, Triethyl citrate (TEC) alone or combination along with the purified hot water to prepare melter mixer stock
b. Stirring and cooling the stock solution
c. Preparing the feed tank using melter mixer stock solution
d. optionally adding additives such as natural colouring agent, synthetic colouring agent, opacifiers, surfactants, super disintegrants, alone or combination which are generally accepted and known or used in the capsule manufacturing industry;
e. Dipping the capsule mould for capsule body and capsule cap in the dip bath
f. Drying and stripping of capsule body and capsule cap from the capsule moulds
g. Cutting the stripped shells and joining of the body part and cap part to form hard empty capsule.
17. The process to prepare hard empty capsule, as claimed in Claim 16, wherein step (e) comprises dip bath temperature at about 65±15°C under constant stirring.
18. The process to prepare hard empty capsule, as claimed in Claim 16, wherein step (e) further comprises pin bar temperature at about 20°C to about 30°C.
19. The process to prepare hard empty capsule, as claimed in Claim 16, wherein step (f) comprises drying of capsule moulds coated with stock solution and thereafter stripping off the shells and cutting to appropriate size to form capsule body part and capsule cap part and joining them to form the hard empty capsule.