Description:FORM 2
THE PATENTS ACT, 1970
(39 OF 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See section 10; rule 13)
1. Title of the invention – A METHOD FOR CLEANING RUBBER CLOSURES

2. Applicant(s)
(a) NAME : Mr. Jagdishbhai Bhagwanbhai Patel
(b) NATIONALITY: INDIAN
(c) ADDRESS: Universal Medicap Ltd.
Survey No. 27/1,28/1, 27/2,28/2,26/1,30 Paikee 1, Rania, Savli, Vadodara-391780
3. PREAMBLE TO THE DESCRIPTION

The following specification particularly describes the invention and the manner in which it is to be performed.

A METHOD FOR CLEANING RUBBER CLOSURES

FIELD OF THE INVENTION

The present invention relates to a method for cleaning rubber closures. More particularly, it relates to a washing and cleaning procedures for pharmaceutical closures using Ozone medium for possible reduction of impurities and extractable from rubber closure.

BACKGROUND OF THE INVENTION

Rubber stoppers are an integral part of pharmaceutical and medical packaging, serving as seals for vials, syringes, and other containers. Maintaining their cleanliness and sterility is important to prevent contamination of pharmaceutical formulations and sensitive medical substances. Traditional methods of cleaning rubber stoppers involve chemical agents and rinsing processes, which can leave behind residue or cause problems in completely removing contaminants.

The current rubber stopper, is commonly used in the sealing of medical or pharmaceutical containers due to its high resilience and ability to provide functions such as effective sealing, gas containment, and protection against contamination of container contents. However, the production process involves multiple steps, including mixing, molding, sulfuration, die-cutting, deburring, checking, and packing, leading to the surface of the rubber stopper easily accumulating various insoluble impurities and particulates during each procedure handover. To ensure the cleanliness of medical or pharmaceutical containers and prevent the contamination of fine particles detrimental to human health, rubber stopper undergo a washing procedure before final packing.

The current cleaning methods primarily involve two approaches: roller and basket-hanging.

One such invention is disclosed in Patent “CN1530179A” Titled – “Cleaning processing method and apparatus for medical or medicinal rubber stopper”. The invention relates to a method and equipment for washing the medical or medicinal rubber plugs features that the high-pressure liquid stream is used to flush said rubber plugs downward, so the rubber plugs are cleaned in semi-suspended or suspended state. Its equipment is composed of container with multiple water spraying holes on its bottom and side wall, washing drum, water storage, water inlet pipe, water outlet pipe, and the pressurizing pump and pressure regulating valve for spraying the cleaning liquid from water spraying holes.

Another such invention is disclosed in Patent “WO1997048754A1” Titled – “A method of cleaning or purifying elastomers and elastomeric articles which are intended for medical or pharmaceutical use”. The invention relates to a method of cleaning or purifying elastomers and elastomeric articles which are intended for medical or pharmaceutical use comprises (a) performing a first solvent extraction process on the elastomer or elastomeric article using a first solvent so as to substantially remove impurities from the elastomer or elastomeric article; (b) subjecting the elastomer or article to a second solvent extraction process using a second solvent to substantially remove residues of said first solvent remaining in the elastomer or article after said first solvent being compatible with the intended medical or pharmaceutical use of the elastomer or article and said second solvent being used at a temperature below its critical temperature; and thereafter (c) drying the elastomer or article.

The roller method employs a rotating drum within a container holding water or cleaning solution, where the rubber stopper is placed. The rotation of the drum in water or cleaning solution aims to achieve cleaning. However, this method has drawbacks, including uneven impurity content and density in the water or cleaning solution, friction-induced particulate generation when rubber stopper come into contact during drum rotation, and the potential for recontamination despite water or cleaning solution reflux and filtration.

The basket-hanging method involves several containers holding clear water or cleaning solution arranged side by side. Rubber stoppers are hung individually in baskets and moved through each container for washing and cleaning. While this method avoids friction and repeated contamination of cleaning fluid, it has its limitations. Rubber stoppers immersed in cleaning fluid under static conditions result in suboptimal cleaning performance, and there is inconsistency in cleaning effectiveness between the center and border areas of the hanging basket, particularly at the zone line where effective washing of rubber stoppers is challenging.

To overcome the said problem raised due to the above mentioned techniques of washing the rubber, the inventor of the present invention come up with the inventive method to washing the rubber stopper with the ozonisation. Ozone, a triatomic form of oxygen with strong oxidizing properties, is widely recognized for its ability to sanitize and disinfect various surfaces. Its application in the field of rubber stopper cleaning offers a promising alternative to conventional methods. Ozone not only effectively eliminates microorganisms, bacteria and fungi, but also decomposes organic and inorganic residues without leaving harmful by-products.

OBJECTIVES OF THE INVENTION

The principle objective of the present invention is to overcome many of the disadvantages of prior art technologies by providing a method for cleaning rubber closures.

Yet another objective of the present invention is to provide a method for cleaning rubber closure which avoids blooming of particles in rubber stopper.

Yet another objective of the present invention is to provide a method for cleaning rubber closure that provides an effective washing & cleaning procedures for pharmaceutical closures using ozone medium for possible reduction of impurities and extractable from finished product.

Yet another objective of the present invention is to provide a method for cleaning rubber closure in which contamination level has been reduced below to an acceptable limit.

Yet another objective of the present invention is to provide method for cleaning rubber closure with ozone that being capable of removing of any presence of contaminant or leachable in rubber closures.

SUMMARY OF THE INVENTION

This summary is provided to introduce a selection of concepts in a simplified form that are further disclosed in the detailed description of the invention. This summary is not intended to identify key or essential inventive concepts of the claimed subject matter, nor is it intended for determining the scope of the claimed subject matter.

The present invention is all about a method for cleaning rubber closure with the ozonization.

The main aspect of the present invention is to provide method for cleaning rubber closures, comprising the steps of:
a. dispensing raw rubber and other materials;
b. intermixing or mixing the raw rubber along with other materials;
c. cutting rubber sheets into piles with defined weight after washing;
d. conducting metal detection on the rubber piles;
e. molding the rubber piles to form stopper followed by punching and trimming;
wherein, after completion of punching and trimming, the rubber stoppers are washed with raw water and RO water and the rubber stoppers are treated with 20gm ozone generation for a duration of 10 minutes for ozonization.

DETAILED DESCRIPTION OF THE INVENTION

Detailed embodiments of the present invention are disclosed herein, however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which may be embodied in various forms. Therefore, specific functional and structural details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed structure.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention belongs.

The objects, features, and advantages of the present invention will now be described in greater detail. Also, the following description includes various specific details and is to be regarded as merely exemplary. Accordingly, those of ordinary skill in the art will recognize that: without departing from the scope and spirit of the present disclosure and its various embodiments there may be any number of changes and modifications described herein.

It must also be noted that as used herein and in the appended claims, the singular forms "a", "an," and "the" include plural references unless the context clearly dictates otherwise. Although any systems and methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present invention, the preferred, systems are now described.

The main embodiment of the present invention is to provide a method for cleaning rubber closure.

Throughout the invention, the term “Ozonization” is basically the process of treating something with ozone, which is a molecule made up of three oxygen atoms. It's used for various purposes, like purifying air and water, as ozone has strong oxidizing properties that can help break down or neutralize pollutants.

Throughout the invention, the term “sparger” is a device or apparatus used to introduce or disperse a gas, often for the purpose of cleaning or treating materials. In the rubber stopper cleaning process, the sparger is employed during a specific stage, possibly for washing and treating the rubber stoppers.

Throughout the invention, the term “sparger process” is the use of the sparger device to introduce various substances such as raw water, reverse osmosis (R.O) water, and possibly ozone (Ozonisation) for cleaning and treating the rubber stoppers. This process aims to ensure the cleanliness and sterility of the rubber stoppers, making them suitable for their intended use, possibly in pharmaceutical or medical applications where cleanliness and hygiene are critical.

As per detail embodiments of the present invention, a method for cleaning rubber closures, comprising the steps of:
a. dispensing raw rubber and other materials;
b. intermixing or mixing the raw rubber along with other materials;
c. cutting rubber sheets into piles with defined weight after washing;
d. conducting metal detection on the rubber piles;
e. molding the rubber piles to form stopper followed by punching and trimming;
wherein, after completion of punching and trimming, the rubber stoppers are washed with raw water and RO water and the rubber stoppers are treated with 20gm ozone generation for a duration of 10 minutes for ozonization.

As per detailed embodiment of the present invention, said method further comprising:
a. post shorting and inspection of rubber stoppers;
b. specialized washing of rubber stoppers in a dedicated area for ready-for-sterilization (RFS) or ready-for-use (RFU);
c. packaging of the rubber stoppers; and
d. sterilization of the rubber stoppers.

As per detailed embodiment of the present invention, said rubber closures being used for parenteral pharmaceutical preparations for stoppering drug vials.

As per detailed embodiment of the present invention, after completing the ozonization step, samples of the rubber stoppers being withdrawn, and a reducing substance test is performed; wherein the results of the reducing substance is in the range of 0.70 to 2.00.

As per one embodiment of the present invention, the materials include samples of rubber closures with different rubber types and compound compositions, Ozone generator, and Raw water/R.O. Water/purified water/water for injection.

In accordance with one embodiment of the present invention, the comprehensive production cycle extends until the punching stage, where the punched rubber stoppers progress to the subsequent sparger process. The sparger washing commences with an initial treatment involving raw water, followed by R.O water, accompanied by appropriate treatments as required. Following the sparger treatment, secondary washing and cleaning cycles are executed in accordance with standard procedures. Subsequently, upon the completion of the washing and cleaning protocols, the stoppers undergo Ozonisation as part of the sparger process. Specifically, after the raw water washing cycle, the R.O water sparger cycle involves Ozonisation for a specified duration. Post this Ozonisation phase, secondary washing and cleaning cycles are once again implemented in accordance with established processes.

The present invention was experimented and illustrated more in details in the following example. The example describes and demonstrates embodiments within the scope of the present invention. This example was given solely for the purpose of illustration and is not to be construed as limitations of the present invention, as many variations thereof are possible without departing from spirit and scope.

As per one embodiment of the present invention, the primary objective is to validate the washing procedure for rubber closures using ozone as a medium. This validation aims to reduce the potential extraction of impurities or contaminants, thereby ensuring the safety, efficacy, and quality of the final product. For this Validation procedure, the goal is to demonstrate that the materials have been effectively cleaned, and the contamination levels have been reduced below acceptable limits.

Sr. No. Sample Lot No. Sample Withdraw (A)
Before Reducing Substance (B)
Final result Reducing Substance
(Limit = < 2.0) C=A-B
Difference
Reducing Substances
1 32 mm Grey Bromobutyl 230764 A Sparger 2.00 1.90 0.10
2 32 mm Grey Bromobutyl 230764 B Sparger 2.20 1.70 0.50
3 32 mm Grey Bromobutyl 230764 C Sparger 2.05 1.75 0.30
4 20 mm Slotted Grey Bromobutyl 230919 A Sparger 1.80 1.10 0.70
5 20 mm Slotted Grey Bromobutyl 230919 B Sparger 1.85 1.05 0.80
6 13 mm Semi Slotted Grey Bromobutyl 230950 C Sparger 1.90 1.25 0.65
7 13 mm Gery Bromobutyl 230940 A Sparger 2.20 1.50 0.70
8 20 mm Gery Bromobutyl 231005 A Sparger 1.85 1.30 0.55
9 32 mm Gery Bromobutyl 231012 A Sparger 1.85 1.25 0.60
10 32 mm Gery Bromobutyl 230976 B Sparger 1.80 1.30 0.50
11 13 mm Gery Bromobutyl 230977 A Sparger 2.05 1.65 0.40
12 13 mm Slotted Gery Bromobutyl 230990 C Sparger 2.20 1.70 0.50
13 20 mm Gery Bromobutyl 231021 C Sparger 2.05 1.50 0.55
14 20 mm Gery Bromobutyl 230987 A Sparger 1.35 0.90 0.45
15 20 mm Gery Bromobutyl 230987 B Sparger 2.50 1.10 1.40
16 20 mm Gery Bromobutyl 230987 C Sparger 1.50 1.30 0.20
17 20 mm Gery Bromobutyl 231000 A Sparger 1.30 0.80 0.50
18 13 mm Slotted Gery Bromobutyl 230948 C Sparger 1.25 0.85 0.40
19 32 mm Gery Bromobutyl 230964 B Sparger 1.10 0.70 0.40
20 20 mm Gery Bromobutyl 231009 C Sparger 2.70 1.55 1.15
21 32 mm Gery Bromobutyl 230890 A Sparger 2.25 1.35 0.90
22 32 mm Gery Bromobutyl 230869 A Sparger 2.05 1.45 0.60
23 13 mm Gery Bromobutyl 230970 A Sparger 2.05 1.65 0.40
24 32 mm Gery Bromobutyl 231014 C Sparger 1.60 1.50 0.10
25 32 mm Gery Bromobutyl 231032 A Sparger 1.50 1.30 0.20
26 20 mm Slotted Gery Bromobutyl 231011 A Sparger 1.85 1.15 0.70
27 32 mm Gery Bromobutyl 231034 A Sparger 1.90 1.60 0.30
28 32 mm Gery Bromobutyl 231034 B Sparger 1.65 0.75 0.90
29 32 mm Gery Bromobutyl 231047 A Sparger 1.85 1.50 0.35
30 32 mm Gery Bromobutyl 231046 A Sparger 1.90 1.55 0.35
31 32 mm Gery Bromobutyl 231046 B Sparger 1.75 1.60 0.15
32 20 mm Gery Bromobutyl 231052 A Sparger 1.85 1.45 0.40
34 13 mm Slotted Gery Bromobutyl 231036 C Sparger 2.00 1.55 0.45
35 32 mm Gery Bromobutyl SA23163 Sparger 1.60 1.10 0.50

The conclusion based on above data is that there is significant difference in reducing substance results after Ozonisation.

Without further description, it is believed that one of ordinary skill in the art can, using the preceding description and the illustrative examples, make and utilize the present invention and practice the claimed methods. It should be understood that the foregoing discussion and examples merely present a detailed description of certain preferred embodiments. It will be apparent to those of ordinary skill in the art that various modifications and equivalents can be made without departing from the spirit and scope of the invention. , Claims:CLAIMS

We Claim:-
1. A method for cleaning rubber closures, comprising the steps of:
f. dispensing raw rubber and other materials;
g. intermixing or mixing the raw rubber along with other materials;
h. cutting rubber sheets into piles with defined weight after washing;
i. conducting metal detection on the rubber piles;
j. molding the rubber piles to form stopper followed by punching and trimming;
wherein, after completion of punching and trimming, the rubber stoppers are washed with raw water and RO water and the rubber stoppers are treated with 20gm ozone generation for a duration of 10 minutes for ozonization.

2. The method for cleaning rubber closures as claimed in claim 1, said method further comprising:
a. post shorting and inspection of rubber stoppers;
b. specialized washing of rubber stoppers in a dedicated area for ready-for-sterilization (RFS) or ready-for-use (RFU);
c. packaging of the rubber stoppers; and
d. sterilization of the rubber stoppers.

3. The method for cleaning rubber closures as claimed in claim 1, wherein the rubber closures are used for parenteral pharmaceutical preparations for stoppering drug vials.

4. The method for cleaning rubber closures as claimed in claim 1, wherein af-ter completing the ozonization step, samples of the rubber stoppers being withdrawn, and a reducing substance test is performed; wherein the results of the reducing substance is in the range of 0.70 ml to 2.00 ml.

Date this 13th January 2024