FORM 2

THE PATENTS ACT, 1970
(39 of 1970)
COMPLETE SPECIFICATION
[See section 10]
A PROCESS FOR MANUFACTURING HIGH

1 REFLECTANCE SOLUBLE CONTAINERS';

SCITECH CENTRE, A COMPANY INCORPORATED UNDER SECTION 25 OF THE COMPANIES ACT, 1956, WHOSE ADDRESS IS 7, PRABHAT NAGAR, JOGESHWARI (WEST), MUMBAI - 400 102, MAHARASHTRA, INDIA;



Original
848/MUM/2001
5/9/2009

THE FOLLOWING SPECIFICATION
PARTICULARLY DESCRIBES AND
ASCERTAINS THE NATURE OF THE INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFOMED.
10-10-2006

FIELD OF INVENTION
This invention relates to the preparation of glossy soluble containers and process for their manufacture.
BACKGROUND ART
In manufacture of soluble containers e.g. capsules opacifiers such as titanium dioxide are used to produce controlled opaqueness in the capsule shells. This is done to protect the contents of the containers from direct heat and light. A high reflecting surface is desirable as it can provide enhanced protection to any ultra photosensitive ingredients in formulated products in the containers.
However it is already well known in the art to employ HPMC and starch for manufacturing containers such as capsules. The conventional gelatine can also be replaced by any of the following or any combination of some or all of them; Ethyl cellulose, carboxy methyl cellulose, hydroxy propyl methyl cellulose, polyvinyl alcohol, methacrylic acid copolymers, starch, gums like tragacanth, guargum, acacia & the like.
Methods for manufacturing containers like capsules with gelatine and other materials are known in the art. Such well known methods are known to comprise the steps of melting the gelatine in water by heating and stirring which is followed by the addition of additives like preservatives, plasticizers, colourants, sweeteners & flavouring agents and the like and consequently adjusting the viscosity of the gelatine solution by adding warm water which is followed by de-aeration and the de-aerated gelatine solution with the additives are being transferred to

"cap & body" dipping tank known in the art wherein further conventional steps are employed for manufacturing capsules. Such capsules consist of bodies & caps.
OBJECTS OF THE INVENTION
An object of this invention is to provide a means of enhancing the reflectance of the surface of soluble containers, specifically in the case of gelatine based containers such as capsules by incorporation of gloss
agents to obtain containers such as capsules with uniform reflecting surfaces.
Another object of this invention is to produce containers such as capsules with high reflecting coloured surfaces.
Yet one of the objects of the invention is to reduce or replace the use of titanium dioxide as opacifier and at the same time achieve enhanced
reflectance of containers such as hard capsule shells.
According to another aspect of the present invention the same provides for manufacture of high reflectance containers such as hard capsules for drug / pharmaceutical contents and the like comprising :
- selecting the appropriate gloss agents and providing the same in desired particle size range;
providing the gelatine solution with or without additives in substantially clean form in container / tanks;
adding the gloss agent in said tank;

de-aeration of the solution and providing the same in dipping tank;
dipping the capsule making pin moulds in the solution followed by withdrawing and subjecting the same to drying.
In the present invention various commercially avaiJatel© potassium aluminiunT,jj|icate-coated with titanium dioxide and their like ip- specified particle size range is used to prepare containers such as hard gelatine capsule shells. This pigmented matrix not only gives a lustrous finish to the hard gelatine capsule shells but also helps to eliminate the use of titanium dioxide separately to produce opacity in the containers such as capsules.
SUMMARY OF THE INVENTION
In accordance with a preferred aspect, the process of manufacture of hard capsule shells with gloss involves the following stages :
i. Selection of the gloss agents in the appropriate particle size
range from about 2 microns to about 200 microns.
ii. Making of gelatine solution of about 25% to about 40% w/v in
water.
iii. Addition of preservatives.
iv. Heating of the whole mass with stirring to melt the gelatine to
form a transparent solution. This solution is filtered to remove any extraneous matter and transferred to the gelatine holding tanks.

V. Addition of the gloss agent of about 0.25% w/w to about 10% w/w
preferably between 0.3 to 2% w/w to the gelatine solution as such or in slurry form to prevent any lump formation. Stirring for not less than 5 minutes is done to prevent any lumping. Gelatine solution temperature is maintained in the range of about 40°C to about 65°C, preferably 45 to 55°C.
vi. Incorporation of colourant in a slurry if required to get metallic
coloured shells.
vii. Adjustment of the viscosity of the gelatine solution by addition of desired quantity of warm water.
viii. Addition of natural or synthetic plasticizer in the gelatine solution may be necessary under some conditions.
ix. De-aeration of the solution prior to taking it for capsule formation.
X. Transferring of the solution to the "cap and body" dipping tank.
The temperature of the dipping tank is maintained at about 45°C to about 55°C preferably between 46 to 52°C.
xi. Dipping of the capsule-making pin moulds into the gelatine
solution. The pins are then withdrawn, turned and pushed inside the drying zone. Capsule pins with gelatine on it travel through a drying zone of temperature about 22°C to about 30°C, preferably between 24°C to 28°C. During this time the gelatine is set on the pins and dried.
xii. Mechanical removal of the capsules from the pins.

xiii. The capsules are cut into required length mechanically/^joihed cap and body and kept for aeration at 20°C to 30°C, preferably.24°C to 28°C for 60 minutes to 200 minutes.
The moisture content of the capsules is usually maintained between about 12% to about 20% and most commonly between 15% to 18%.
DETAILED DESCRIPTION OF THE INVENTION
In accordance with a preferred aspect, the process of manufacture of hard capsule shells with gloss involves the following stages :
i. Selection of the gloss agents in the appropriate particle size
range from about 2 microns to about 200 microns.
ii. Making of gelatine solution of about 25% to about 40% w/v in water.
iii. Addition of preservatives.
iv. Heating of the whole mass with stirring to melt the gelatine to
form a transparent solution. This solution is filtered to remove any extraneous matter and transferred to the gelatine holding tanks.
V. Addition of the gloss agent of about 0.25% w/w to about 10% w/w
preferably between 0.3 to 2% w/w to the gelatine solution as such or in slurry form to prevent any lump formation. Stirring for not less than 5 minutes is done to prevent any lumping. Gelatine solution temperature is maintained in the range of about 40°C to about 65°C, preferably 45 to 55°C.

vi. Incorporation of colourant in a slurry if required to get metallic
coloured shells.
vii. Adjustment of the viscosity of the gelatine solution by addition of
desired quantity of warm water.
viii. Addition of natural or synthetic plasticizer in the gelatine solution may be necessary under some conditions.
ix. De-aeration of the solution prior to taking it for capsule formation.
X. Transferring of the solution to the "cap and body" dipping tank.
The temperature of the dipping tank is maintained at about 45°C to about 55°C preferably between 46 to 52°C.
xi. Dipping of the capsule-making pin moulds into the gelatine
solution. The pins are then withdrawn, turned and pushed inside the drying zone. Capsule pins with gelatine on it travel through a drying zone of temperature about 22°C to about 30°C, preferably between 24°C to 28°C. During this time the gelatine is set on the pins and dried.
xii. Mechanical removal of the capsules from the pins.
xiii. The capsules are cut into required length mechanically, joined cap and body and kept for aeration at 20°C to 30°C, preferably 24°C to 28°C for 60 minutes to 200 minutes.
The moisture content of the capsules is usually maintained between about 12% to about 20% and most commonly between 15% to 18%.
The process will now be described with a set of non-limiting examples.

Example 1.
165 g. of gelatine was weighed in a beaker 335g of deminaralised water was added. The mass was heated on a water bath at 50°C to 60°C with constant stirring so that the gelatine dissolves completely. 2.5g. of the potassium aluminum silicate coated with titanium dioxide in the particle
size range 5 microns to 30 microns was added directly or mixed with water into the gelatine solution and stirred well. The entire mass was de-aerated at 50°C for one hour. Capsule moulding pins cap and body were hand dipped and dried in the capsule drying zone. After drying the capsules were removed from the pin.
Example 2.
165 g. of gelatine was weighed in a beaker 335g of deminaralised water was added. The mass was heated on a water bath at 50°C to 60°C with constant stirring so that the gelatine dissolves completely. 5 g. of the potassium aluminum silicate coated with titanium dioxide in the particle size range 5 microns to 30 microns was added directly into the gelatine solution and stirred well. The entire mass was de-aerated at 50°C for one hour. Capsule moulding pins cap and body were hand dipped and dried in the capsule drying zone. After drying the capsules were removed from the pin.
Capsules formed by this process have moisture content of 13% w/w and disintegration time of 3-4 minutes in water as per pharmacopoeial method.
Reflectance of films were measured and compared against standards.

Reflectance Measurements.
Reflectance was measured on a Gretag Macbeth (UK) - Model CF 2180 colour-matching system equipment.
33.3g. of dry gelatine was weighed and 66g water was added. It was heated on a water bath around 55°C to make gelatine solution. Once the gelatine was solubilised it was filtered to give a clear transparent solution. This solution was spread evenly on a glass plate. The film was dried in the capsule-drying zone for 2 hrs. The film was removed from the glass plate and cut into 2-inch square pieces. The reflectance was measured against whiteand black background at 31 points from 400 nm to 700 nm on the colour-matching instrument.
Four samples were independently prepared with the addition of : a) 0.25 g. of gloss agent; b) 0.25 g. of titanium dioxide; c). 1.0 g. of gloss agent; d). 1.0 g. of titanium dioxide.
The results of the reflectance measurements are given in table 1.
% Reflectance of the capsule shell with the gloss is higher as compared a capsule shell with the same quantity of Ti02.
This establishes the enhanced reflective character of the capsules prepared with the gloss agent materials. The high reflectance also shows that additional Ti02 is not necessary to achieve the required opacity in the capsule shells.

The following observations are of significance :
■ The percentage reflectance shows that against black and white
background the film made with gloss agent shows more reflectance
compared to the film prepared with only titanium dioxide.
■ Films prepared with 0.25% of both the materials when compared
for reflectance data against white background shows that the gloss agent
has 5% to 20% higher reflectance in the range of 400 to 700 nm.
■ Films prepared with 0.25% of both the materials when compared for reflectance data against black background shows that the gloss agent has 5% to 12% higher reflectance in the range of 400 to 700 nm.
■ Films prepared with 1% of both the materials when compared for reflectance data against black background shows that the gloss agent has 26% to 29% higher reflectance in the range of 400 to 700 nm.
■ Surprisingly films prepared with 1% of both the materials when
compared for reflectance data against white background shows that the
gloss agent has 1 % to 3% lower reflectance in the range of 400 to 700
nm.
The capsule shells prepared by the method of this invention followed and showed the same trend in the reflectance as described above.
Another surprising finding is that the capsules prepared with the addition of the gloss materials were tested for their shrinkage properties. They were found to be more resistance than the capsules prepared without these materials. The capsules so prepared did not need the addition of

opacifiers such as titanium dioxide that is normally required in opaque capsule shell making.
Table 1 : Comparative Reflectance measurements on samples with Ti02 and with only the gloss agent at various levels.

Gloss Gloss Gloss Gloss
agent Ti02 agent Ti02 Agent Ti02 Agent Ti02
NM 0.25% white 0.25% white 0.25% black 0.25% black 1% white 1% white 1% black 1% black Only gelatine Black back-ground
400 80.28 58.47 32.77 20.74 62.04 65.19 56.61 28.04 12.96
410 82.91 62.79 32.98 21.57 64.93 69.18 58.11 28.80 12.97
420 84.56 65.92 32.92 21.96 66.97 71.70 58.73 29.02 12.88
430 85.98 68.78 32.74 22.54 68.92 74.13 59.43 29.47 13.02
440 86.64 70.86 32.40 22.76 70.48 75.73 59.72 29.55 12.92
450 87.59 73.06 32.11 23.04 71.99 77.40 60.01 29.67 12.96
460 88.38 75.00 31.75 23.20 73.48 78.83 59.94 29.67 12.93
470 89.13 76.83 31.33 23.44 74.87 80.22 60.04 29.76 12.90
480 89.68 78.36 30.88 23.52 76.15 81.21 59.69 29.70 12.89
490 90.13 79.67 30.51 23.55 77.20 82.18 59.50 29.64 12.86
500 90.54 80.90 30.16 23.68 78.19 83.12 59.43 29.68 12.87
510 91.00 81.89 29.79 23.66 79.05 83.84 59.16 29.57 12.84
520 91.16 82.51 29.38 23.56 79.86 84.26 58.82 29.41 12.83
530 91.28 82.93 28.99 23.44 80.46 84.49 58.28 29.15 12.77
540 91.68 83.52 28.68 23.36 81.19 84.92 58.14 29.01 12.74
550 91.81 84.14 28.40 23.38 81.83 85.41 57.96 29.01 12.77
560 91.91 84.66 28.15 23.30 82.36 85.76 57.69 28.84 12.79
570 91.91 84.96 27.97 23.22 82.89 85.96 57.48 28.71 12.80
580 92.00 85.18 27.72 23.07 83.24 86.05 57.28 28.50 12.75
590 92.00 85.43 27.50 22.98 83.60 86.25 57.04 28.30 12.77
600 92.18 85.67 27.31 22.87 83.91 86.46 56.81 28.17 12.76
610 92.46 86.00 27.21 22.76 84.31 86.66 56.71 28.00 12.82
620 92.41 86.05 27.13 22.69 84.44 86.67 56.61 27.80 12.86
630 92.39 86.23 26.98 22.49 84.67 86.82 56.37 27.57 12.79
640 92.43 86.50 27.01 22.46 85.14 87.07 56.36 27.48 12.83
650 92.62 86.67 26.98 22.46 85.36 87.17 56.32' 27.39 12.97
660 92.78 86.66 26.93 22.35 85.58 87.18 56.19 27.20 13.14
670 92.84 86.88 27.32 22.58 85.78 87.35 56.22 27.36 13.55
680 92.69 86.78 27.67 22.84 85.97 87.14 56.02 27.45 14.23
690 92.73 86.81 28r70 23.78 86.07 87.21 55.99 28.02 15.65
700 92.89 86.99 30.47 25.33 86.38 87.42 56.10 29.45 18.10

8. The high reflectance soluble containers as claimed in claim 6 wherein the gloss agent is preferably present in an amount 0.3% to 2% w/w of the gelatin solution.
9. The high reflectance soluble containers as claimed in claim 6 wherein the capsules contain the moisture in the range 12% to 20% and preferably 15% to 18%.
10. The high reflectance soluble containers as claimed in claim 6 wherein the capsules have improved shrinkage resistant properties.
Dated this 5th day of September, 2001
FOR SCITECH CENTRE
By their Agent

(MANISH SAURASTRI) KRISHNA & SAURASTRI