Abstract: The present invention relates to an herbal flavoured tea composition and a process for its manufacturing. The process of manufacture provides four variant compositions of herbal flavoured tea by using four combinations of herbal flavours. The combinations of herbal flavours include herbs like Bacopa monnieri, Ocimum sanctum, Mentha piperita etc. The process involves blending of flavour concentrate with Darjeeling Brokens and plain bulk tea. The flavour concentrate is made by preparing an emulsion by adding an encapsulant in water, adding natural flavours, spraying the emulsion of natural flavours onto 10-50% of the tea used in formulation followed by gentle and rapid drying in a fluidised bed drier. The herbal flavoured tea composition manufactured by the process has unique texture, taste like tea and has higher shelf life stability. The modification of the final taste of the final tea product can be achieved by adjustment during the dilution/ blending stage.
Field of Invention
This invention relates to an herbal flavoured tea composition and process of manufacturing thereof wherein natural herbal flavours are coated on to a definite proportion of tea using an encapsulant/binder, followed by mixing & rapid drying at low temperature to retain flavour actives and tea flavour and diluting/blending the flavour concentrate thus produced with tea in right proportion.
Prior Art
Knowledge from Traditional Indian Medicine System (TIMS) "Ayurveda" has been used to produce a new range of tea products with do-good ingredients from herbs. Since, black tea is consumed more; the new tea products and processes have been evolved mainly on black tea matrix. However, other tea matrix can also be used in such products and processes. Manufacturing process of making black tea as known in the art involves, plucking of green leaves from the plant Camellia sinensis and then subjecting them to withering (partial removal of moisture) followed by fermentation (exposes polyphenols to enzymes, causing their oxidation to various coloured products) and then fired (Dried to complete moisture removal).
The plucked tea-leaves have a moisture content of 70-80% and are withered by storing them in big containers or withering troughs. In this holding step some moisture is lost and senescence occurs. The product is then chopped and reduced in size by a distorting unit called rotorvane. More reduction and initiation of fermentation happens during cutting in CTC (crush-tear-curl). Fermentation takes place at moisture contents between 55-75%. From this moisture content, the product is dried in a fluidised bed dryer till final moisture content of 2-3%. Next the product is cleaned, graded and bulked followed by packing and shipping.
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Among all the unit operations mentioned above, drying is the most important unit operation in tea manufacturing process. Major functions of drying are -inactivation of enzymes to arrest fermentation, reduction of moisture to increase the shelf stability of black tea and development of black tea character and flavour. Being a vegetable material, tea is hygroscopic in nature with skeleton of the material consisting of cells in which networks of very fine capillaries exist.
After the instationary heating, drying continues by evaporation of surface moisture. The evaporation takes place at a constant rate which is determined by external conditions: temperature of the air, hydrodynamic conditions of the air, surface area and relative humidity. The rate can be increased by applying higher psychrometric difference thereby increasing the temperature or humidity difference between product and air, increasing the amount of air in contact with the product or increasing the surface area of the product in contact with the air. Basically during this phase, the evaporation rate is controlled by the diffusion of vapour through the product/air interface. During this period the diffusion rate in the product is sufficiently high to maintain a water activity close to one at the surface. The temperature of the surface takes approximately the wet-bulb temperature. After some time dry spots arise at the surface of the product and water activity drops below one.
Next phase of drying is the falling rate period. During this phase, drying rate is determined by the internal conditions inside the product. Temperature of the product rises to the temperature of drying air. The free moisture in the capillaries evaporates and the residual bound moisture exerts a low vapor pressure as shown in Fig 1. The last bound water can be removed if the relative humidity of the drying air is lower than the water activity in the micropores.
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In the herbal tea products known in the art and their processes for manufacturing, the raw herbs are mixed with the black tea in desired proportions to obtain the desired herbal tea products.
A drawback of the above processes used in the known art for manufacturing herbal tea products is that these processes involve mixing of untreated dried herbs which could be harmful, since most of the herbs are either sun or shade-dried and are often contaminated with pests and microbes which may cause serious illness to the consumers of such herbal tea products.
Another drawback of the above processes known in the art for manufacturing herbal tea products is that the method for treatment of raw herbs used in these processes involves exposing the herbs to the source of ionizing radiation in the form of gamma ray from Cobalt - 60 irradiation source or subjecting the raw herbs to fumigation by a fumigant like ethylene oxide. The gamma ray method is expensive and also involves the possible risk of inducing radioactivity in herbs. Products using gamma irradiation need to have a label declaration as per the current legislation, which is a trade barrier. Whereas, the fumigation method has the risk that the traces of fumigant may be left on the herbs which may cause health hazards to the consumers of such herbal tea products? Due to these reasons, these techniques are usually not recommended for the treatment of raw herbs.
Still another drawback of the above processes known in the art is that herbs can be added at various steps of black tea manufacture viz., withering, fermentation and drying, which leads to sensory problems like distorted tea taste, off notes generation and faded end cup colour. Apart from sensory issues, it also creates physical problems like non-uniform blends, separation of herbs and tea particles in the final product because of varying size and density.
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Indian Patent Application No. 1317/DEL/2003 discloses a process of manufacturing herbal tea granules. The process involves reacting herbs with water/milk at a temperature of 40-50° C and separation of liquid portion followed by concentrating mass under controlled temperature and vacuum to attain total soluble solids (TSS) of about 80-85%. Inactive nutritive components, palatable enhancers and solubility enhancers are mixed to the above concentrated mass, which is optionally followed by addition of natural binders. Concentrated mass having a TSS of 80-85% is mixed using conventional methods to tea and forming a thin layer of the above mass into trays with thickness not more than 2 cm and dried in vacuum drier at temperature 50-60 °C for about 2h. The herb taken is like Gurmar and the extract is prepared by coarse grinding, solvent extraction with milk and water in hot water and concentration. The binder used is a natural binder like Psyllium husk mucilage
A drawback of the above process is that the herbal tea product is hygroscopic in nature.
Indian Patent Application No. 279/CHE/2004 discloses a novel herbal tea for diabetes & obesity. The composition is a blood purifier that can purify the toxins in the blood. The process of preparation involves mixing of nine herbs with tea.
Indian Patent application No. 916/CHE/2004 relates to herbal tea which has specific properties of reducing cholesterol in the humans upon consumption. The composition is prepared by mixing certain herbs with tea powder.
A drawback of the above processes is that in these processes raw herbs are used due to which the final appearance of the herbal product obtained by the process has texture and taste different from the tea.
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Another drawback of the above processes is that as the raw herbs are used in these processes there is risk of contamination/infestation due to the reason that the raw herbs are generally shade dried or sun-dried during which there is risk of contamination/infestation by pests which may be health-hazardous.
Objects of the Present Invention
The primary object of the present invention is to provide an herbal flavoured tea composition and process for its manufacturing using herbal flavours.
Another object of the present invention is to provide a novel herbal tea composition with do-good ingredients in the form of natural flavours and orthodox tea from Darjeeling referred to as 'Darjeeling Brokens'. The Darjeeling Brokens, which are bright green in colour, give this product a unique texture, which is very different from available regular black tea.
Still another object of the present invention is to provide a process of making flavoured herbal tea, wherein in the final product is made in two main steps comprising first step of making of flavoured concentrate and the second step of dilution/blending with tea or tea components to get the final product.
Yet another object of the present invention is to provide a process for manufacturing herbal flavoured tea composition wherein herbal flavour extracts are used in lieu of raw herbs used in the processes known in the art thereby avoiding the possible risk of contamination/infestation by pests or microbes which arises in the use of raw herbs which are shade-dried or sun-dried. This ensures the product quality and safety from causing any health hazards to consumers.
Still another object of the present invention is to provide a process for manufacturing herbal flavoured tea composition wherein the herbal extracts are
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generally incorporated in about 10 % of the base blend with subsequent drying and blending with bulk tea due to which the final product has a taste like the taste of normal tea.
Further object of the present invention is to provide a flavoured herbal tea product wherein flavour delivery can be increased or decreased by regulating the ratio between flavour concentrate and tea during dilution/blending. This allows modification of final taste of the final tea product by adjustment during the dilution/blending stage.
Still further object of the present innovation is to provide a process which utilises Darjeeling Brokens which are manufactured from Darjeeling tea leaves without the procedure of 'cut, tear and crush' (CTC) of tender tea leaves.
Yet further object of the present invention is to provide a process wherein the flavoured concentrate made by coating flavours on 10-50% of the black tea, appears similar to the black tea. Due to this reason, the final product obtained by blending the flavoured concentrate with tea, the segregation between flavoured coated tea leaves and uncoated tea leaves is not observed and the final product appears as a uniform homogenous product with absolute synergy between the ingredients both in terms of texture as well as taste.
Even further object of the present invention is that it provides a 'flavour concentrate' which when diluted/blended with the tea or other tea components gives a flavoured tea, which can be made with or without milk.
Yet further object of the present invention is to provide a process for manufacturing herbal flavoured tea product wherein flavour extracts are added along with a binder thereby the flavour concentrate is protected from deterioration
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Still further object of the present invention is to provide a process for manufacturing herbal flavoured tea product wherein water soluble flavour extracts having defined specifications are used and hence the product quality is defined.
Even further object of the present invention is to provide a process for manufacturing herbal flavoured tea product wherein the herbal extracts are incorporated through a binder due to which the product is not hygroscopic and therefore the product retains quality over longer periods i.e. the product has higher shelf life stability.
Yet further object of the present invention is to provide a process for manufacturing herbal flavoured tea product wherein all the ingredients used are water soluble which obviates the need for extended brewing which is required in the known processes using raw herbs. This enables the user to brew the tea in a way that is being practical for brewing normal tea.
Statement of Invention
According to this invention, there is provided a flavoured herbal tea composition comprising, as weight percentages of composition: 10-50% of flavour concentrate, 50-90% by weight of plain bulk tea, 1 to 8% by weight of Darjeeling Brokens, which is orthodox smaller or broken leaf grade of Darjeeling tea, wherein further flavour concentrate comprises 0.5 -5% by weight of natural herbal flavours, 0.3 to 0.7 % by weight of an encapsulant and rest as tea particles and wherein further said flavour concentrate is obtained by the steps of:
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(a) preparing an emulsion by adding slowly 0.3 to 0.7% by weight of an encapsulant to hot water at temperature between 60°C and 80°C with mixing in an emulsifier for about 5 minutes till a homogenous solution is obtained; cooling the solution to 40-60°C; adding a combination of different natural herbal flavours selected from Composition-A, Composition-B, Composition-C and Composition-D as hereinafter described, so that the emulsion has a solid content in the range of 40 to 80%, mixing the solution again at rotational speed higher than lOOOrpm for about 10 minutes, obtaining thereby an emulsion, wherein
-said composition-A of herbal flavours includes 0.1 - 0.5% of Bacopa monnierr, 0.3 - 0.7 % of Ocimum sanctum, 0.05 -0.3% of Mentha piperita, 0.05 - 0.3% of Zingiber officinalis and 0.1 - 0.3% of Elettaria cardamomum;
-said composition-B of herbal flavours includes 0.05 - 0.15% of Salvia officinalis, 0.5 - 0.11% of Glycyrrhiza glabra, 0.01-0.09% of Mentha piperita and 0.1 - 0.3% of Zingiber officinalis ;
-said composition-C of herbal flavours includes 0.1 - 0.55 of Bacopa monnieri, 0.05 - 0.15% of Centella asiatica, 0.3 -0.7% of Ocimum sanctum, 0.1 - 0.3% of Zingiber officinalis, and 0.05 - 0.15 of Foeniculum vulgare; and
-said composition-D of herbal flavours includes 0.005 -0.013% of Trachispermum ammi, 0.1 - 0.2% of Mentha piperita, and 0.05 - 0.35% of Elettaria cardamomum;
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(b) wet blending the tea particles with the emulsion as obtained by the step (a) by spraying the said emulsion slowly on to the 10-50% of the tea with mixing in a Foerberg mixer for 5 to 20, preferably 12 to 15 minutes for uniform coating thereby obtaining wet tea agglomerate of tea particles with moisture content between 15 and 30% and homogenously coated with the said emulsion; and
(c) drying the wet tea agglomerate obtained by step (b) above gently but rapidly in a fluidized bed dryer with inlet air temperature of 70-110°C preferably between 80-90°C and residence time of 6-10 minutes, till the moisture content is reduced to 2 to 3%, obtaining thereby flavour concentrate.
According to this invention, there is provided a process for manufacturing flavoured herbal composition comprising the steps of:
(a) Preparation of flavour concentrate by the steps of:
(i) preparing an emulsion by adding slowly 0.3 to 0.7% by weight of an encapsulant to hot water at temperature between 60°C and 80°C with mixing in an emulsifier for about 5 minutes till a homogenous solution is obtained; cooling the solution to 40-60°C; adding a combination of different natural herbal flavours selected from Composition-A, Composition-B, Composition-C and Composition-D as hereinafter described, so that the emulsion has a solid content in the range of 40 to 80% mixing the solution again at rotational speed higher than lOOOrpm for about 10 minutes, obtaining thereby an emulsion, wherein
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-said composition-A of herbal flavours includes 0.1 - 0.5% of Bacopa monniert, 0.3 - 0.7 % of Ocimum sanctum, 0.05 - 0.3% of Mentha piperita, 0.05 - 0.3% of Zingiber officinalis and 0.1 - 0.3% of Elettaria cardamomum;
-said composition-B of herbal flavours includes 0.05 - 0.15% of Salvia officinalis, 0.5 - 0.11% of Glycyrrhiza glabra, 0.01-0.09% of Mentha piperita and 0.1 - 0.3% of Zingiber officinalis ;
-said composition-C of herbal flavours includes 0.1 - 0.55 of Bacopa monnieri, 0.05 - 0.15% of Centella asiatica, 0.3 - 0.7% of Ocimum sanctum, 0.1 - 0.3% of Zingiber officinalis, and 0.05 -0.15 of Foeniculum vulgare; and
-said composition-D of herbal flavours includes 0.005 - 0.013% of Trachispermum ammi, 0.1 - 0.2% of Mentha piperita, and 0.05 -0.35% of Elettaria cardamomum;
(ii) wet blending the tea particles with the emulsion as obtained by the step (a) by spraying the said emulsion slowly on to the 10-50% of the tea with mixing in a Foerberg mixer for 5-20 minutes preferably 12-15 minutes for uniform coating obtaining thereby wet tea agglomerate of tea particles with moisture content between 15 and 30 % and homogenously coated with the said emulsion; and
(iii) drying the wet tea agglomerate obtained by step (b) above gently but rapidly in a fluidized bed dryer with inlet air temperature of 90-110°C and residence time of 6-10 minutes, till the moisture content is reduced to 2 to 3%, obtaining thereby flavour concentrate.
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(c) diluting/blending with 90 to 50% by weight of plain bulk tea and 1 to 8% of Darjeeling Brokens which is orthodox smaller or broken leaf grade of Darjeeling tea, to obtain the desired herbal flavoured tea composition
The present invention provides a novel herbal flavoured tea product in four different variants by choice of the different combination of natural herbal flavours provided in the present invention. The variant compositions of herbal flavoured tea product have distinct appearance and do-good ingredients in the form of natural flavours, with orthodox tea from Darjeeling referred to as 'Darjeeling Brokens'. Added Darjeeling Brokens, which are bright green in colour, give this product a unique texture, which is very different from available regular black tea. The different composition of herbal flavours used to obtain four variant herbal tea products are tabulated in table-1.
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Table 1. Different compositions of herbal flavours used to obtain variant herbal tea products
Brief Description of Figures
The invention is illustrated with accompanying drawings which are intended to illustrate the invention and are not intended to be taken restrictively to imply any limitation on the scope of the present invention. In the accompanying drawings:
Fig.1: Shows convective tea drying with heated air
Fig.2 : Shows comparison of reflectance/colour scores of flavour
concentrates with bulk tea
Fig.3 :Shows sieve analysis results of black tea (TL 01), flavour
concentrate & composition -A
Fig.4 : Shows the flow chart of the process for preparation of falvoured
herbal tea composition of the present invention.
Description of the invention
All percentages of ingredients herein are by weight unless otherwise specified.
By tea is meant black tea, green tea or oolong tea processed from leaf material from Camellia sinensis van sinensis or Camellia sinensis van Assamica. It also includes rooibos tea obtained from Aspalathus linearis. The term tea also includes black tea made by CTC or orthodox methods and blends of two or more teas.
In accordance with this invention, only natural flavours are used in the process. First encapsulant is added slowly to hot water with mixing in Silverson emulsifier for 5 min. As utilized herein, 'hot' or 'hot water' refers to a temperature between 60 °C and 80 °C. The solution is then cooled to 40-60 °C, followed by addition of
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all the flavours with mixing at >1000rpm for 10 min. The process is represented as a flow chart in fig. 4.
Encapsulant herein, is a modified starch derived from waxy maize, known for its ability to form very stable oil-in-water emulsions. The fine particle size of the emulsion results in reduced losses during drying. Also, low viscosity permits the preparation of emulsions at higher solids.
Considering that the added water content will have to be removed later in the process, and will add up to the drying cost, optimized volume of water with 40-80% flavour loading is used.
The solution is subjected to high speed emulsification at high speed rotation >1000 rpm. The high speed rotation of the rotor blades exerts a powerful suction, drawing liquid and solid materials upwards from the bottom of the vessel and into the centre of the workhead. Centrifugal force then drives the materials towards the periphery of the workhead where they are subjected to a milling action in the precision machined clearance between the ends of the rotor blades and the inner wall of the stator. This is followed by intense hydraulic shear as the materials are forced, at high velocity, out through the perforations in the stator and circulated into the main body of the mix. The materials expelled from the head are projected radially at high speed towards the sides of the mixing vessel. At the same time fresh material is continually drawn into the workhead, maintaining the mixing cycle. The effect of horizontal (radial) expulsion and suction into the head is to set up a circulatory pattern of mixing, which is all below the surface. As a result of this kind of mixing action no unnecessary turbulence or frothing is created at the surface. The entire content of the vessel passes hundreds of times through the workhead during the mixing operation to give uniformly homogenized emulsion.
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In addition to the use of powdered natural flavours, liquid flavours (oils)/oleoresins are also be used in the above mentioned process of making emulsion.
The emulsion thus made is then coated on to the tea particles using a mixer having Foerberg design. The emulsion is added to the tea particles as a fine spray through a nozzle using pressure vessel arrangement. During spraying an FDB (flow distortion bar) is used. FDB is a rotor with radial pins. The pins throw the particles at high speed and create a horizontal curtain across the liquid stream. The single particle exposure to the liquid is short and ensures good distribution of the liquid on to the tea particles. The angular paddles of this mixer are welded to the paddle shafts, which give an overlapping rotation in the middle of the mixer and sweeping the entire bottom of the mixer according to the specified clearance. This gives a mixing pattern, which causes a counter clockwise rotational movement along the perimeter of the mixer also called as transport zone and creation of fluidized zone in the centre, where particles have freedom of movement. The overall mixing pattern ensures homogeneous mixing without breaking tea particles.
The wet mass thus obtained is subjected to drying. To prevent oxidative thermal damage of added flavours, drying should be gentle and fast. As mentioned above drying is the most critical unit operation as it determines the texture of tea along with flavour, taste body and other attributes. Volume of water used during emulsification is calculated such that with above said flavour loading when added to 10-50% of tea fraction increases the moisture content up to 30%.
With above said moisture content our product falls into 'falling phase drying' where the rate is determined by internal conditions inside the product, thus diffusion becomes the rate-determining step. The drying conditions are optimized with inlet air temperature of 90-110 °C and residence time of 6-10min. Final
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moisture content in dried 'flavour concentrate' obtained is 2-3%. The fluidized bed dryer used specifically for this process, has following key features:
-Aerodynamic steel fabricated (fully over ground) plenum chamber - This eliminates entire civil work and ensures scientific air distribution for better fluidization. Multiple guide vanes have been provided to further control airflow.
-Variable speed drive - A variable speed drive system enables the user to set the desired drying time.
-Aerofoil design - For maximum efficiency, the hot air fan has been specially designed with aerofoil impeller blades to deliver the required quantum of hot air at lowest power consumption.
-Energy efficient cyclone system - A power efficient cyclone dust extraction system has been specially designed to pick-up only fibre, fluff, leaving the tea particles behind in the chamber.
Other appreciable features were inbuilt feeder and optional pneumatic discharge valve, which is basically a pneumatic chamber with a blower to cool the dryer mouth tea and enables single point collection on either side of the chamber.
Flavour concentrate made is diluted/blended with 90 to 50% of plain bulk tea and 1 to 8% of Darjeeling Brokens to get the product. In the present invention a rotary blender is used for blending, static vertical blender can also be used for the said operation.
The four variant formulations of the herbal flavoured tea product obtained by the use of variant compositions of natural herbal flavours are as under:
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Colour analysis
The flavour concentrate/final product thus made is compared with the reflectance/colour scores of the bulk tea using Hunterlab. As described herein, Hunterlab Ultrascan XE machine uses TTRAN mode (Total Transmittance Mode) or RSEX mode (Total reflection mode) for colour analysis. Integration of reflectance/transmittance values over the visible spectrum gives Tristimulus X, Y and Z values {Refer ASTM E308).
In Hunter scale, L* measures lightness and varies from 100 for perfect white to zero for black, approximately as the human would evaluate it. The chromaticity dimensions (a* and b*) give understandable designation of as follows:
a* Measures redness when positive, gray when zero and greenness when negative.
b* Measures yellowness when positive, gray when zero and blueness when negative.
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Relationship between Hunter lab scale and the International Commission on Illumination, CIE XYZ scale for the CIE 1931 2° Standard observer and the CIE 1964 10° standard observer is as follows:
Where:
X,Y and Z are CIE Tristimulus values.
Xn, Yn and Zn are the tristimulus values of the standard illuminant. Ka and Kb are chromaticity coefficients
The results of the scores are shown in fig 3. For concentrates, 3-4units drop in L* value is fixed, with increment of 0.5-1.0 unit in a* and 0.2 - 0.5 unit in b* value for present formulations under reflectance mode.
Taster Scores
Brew of all the four formulations along with bulk tea (TL01) was prepared as described below for evaluation by tasters.
Method of preparation: 5 g of tea brewed in 250 ml of hot water (90-95°C)
for 5 minutes, strain and add 5ml of preboiled milk.
Tea taster scored the four present formulations along with bulk tea (TL 01). The scores were given in four categories viz.,Colour, Sparkle, Body and Zing.
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Wherein these parameters as described by tasters under a scheme to evaluate
teas numerically refer to:
- Hue or tea colour when made with milk from red to orange to yellow. Depth of
the colour is to be defined by the sparkle attribute.
Sparkle - Intensity of the colour from grey to pure, from dull/dead to alive/rich.
Colour and sparkle work in a matrix. Both parameters are required to plot the tea evaluation characteristics. Colour forms the X axis and sparkle forms the 'Y' axis.
Body - The weight of tea in the mouth. The level of mouth feel vary from watery
to full.
Zing - The overall quality impression of the tea on the palate. It is used to
express how well the individual attributes of the tea come together in the mouth
and also to express how well defined the tea is, in the mouth.
The compiled results are tabulated in table 2.
Table 2. Taster Scores
Particle size analysis
One of the main concerns of this process is reduction in particle size during processing.
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To address this, particle size analysis is done for the base tea, flavour concentrate, and final blended product. The results are tabulated in table 3-5 and the comparative results are shown in Fig.3
Post analysis of results, it was reported that no appreciable change in particle size happens during processing.
Table 4. Sieve analysis - Flavour Concentrate*
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Table 3. Sieve analysis - Bulk tea (TL 01)
Examples
The invention is now illustrated with working examples which are intended to illustrate the working of the invention and are not intended to be taken restrictively to imply any limitation on the scope of the present invention. In the present examples we have shown formulations, wherein, flavour concentrate is diluted with both bulk tea & orthodox tea. Similar kind of product can be made without using orthodox tea. Also, in present examples formulations are made using 40% emulsion loading. Similar products can be made with emulsion loading upto 80%.
Specifications of the natural flavours used are tabulated in table 6.
Table-6: Specification of Natural herbal flavours used in the present invention
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Example 1: Using Composition-A of herbal flavours
For a batch size of 2 kg, the formulation details are mentioned in table 7.
Table 7. Details of Formulation using Compositon - A of Herbal flaovours
10g of encapsulant is added to the 51 ml of hot water with mixing using Silverson emulsifier for 5 min as described elsewhere, till a homogenous solution is formed. This solution is then allowed to cool to 50-60 °C followed by addition of all the flavour (total 24 g) as mentioned in table 6. The resultant solution is then mixed again at 3000 rpm for 10 min to get an emulsion with 40% solids.
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This emulsion is then slowly sprayed on to the 190.6 g of tea (10% of bulk tea) using compressed air at a pressure of 4kg/cm2 and flow rate of 300ml/min in the Foerberg mixer for 12 min. The wet tea agglomerate thus made has approximately 15.47 % (theoretical) moisture content.
The wet tea agglomerate is dried in a Fluid bed drier for 10 min down to 2-3% moisture content. The 'flavour concentrate' thus made is diluted/blended with 1715.4g (1906g-190.6g) with 60g of Darjeeling Brokens in a vertical blender to get the final product.
Example 2 : Using Composition-B of herbal flavours
For a batch size of 2 kg, the formulation details are mentioned in table 8. Table 8. Details of Formulation using Composition - B of herbal flavours
10g of encapsulant is added to the 49.5 ml of hot water with mixing using Silverson emulsifler for 5 min as described elsewhere, till a homogenous solution is formed. This solution is then allowed to cool to 50-60 °C followed by addition of all the flavour (total 23 g) as mentioned in table 7. The resultant solution is then mixed again at 3000 rpm for 10 min to get an emulsion with 40% solids.
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This emulsion is then slowly sprayed on to the 190.7 g of tea (10% of bulk tea) using compressed air at a pressure of 4kg/cm2 and flow rate of 300ml/min in the Foerberg mixer for 12-15 min. The wet tea agglomerate thus made has approximately 14.94 % (theoretical) moisture content.
The wet tea agglomerate is dried in a Fluid bed drier for 10 min down to 2-3% moisture content. The 'flavour concentrate' thus made is diluted/blended with 1716.3g (1907g-190.7g) with 60g of Darjeeling Brokens in a vertical blender to get the final product.
Example 3: Using Composition-C of herbal flavours
For a batch size of 2 kg, the formulation details are mentioned in table 9. Table 9. Details of formulation using Compositon - C of herbal flavours
10g of encapsulant is added to the 51 ml of hot water with mixing using Silverson emulsifier for 5 min as described elsewhere, till a homogenous solution is formed. This solution is then allowed to cool to 50-60 °C followed by addition of all the flavour (total 24 g) as mentioned in table 6. The resultant solution is then mixed again at 3000 rpm for 10 min to get an emulsion with 40% solids.
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This emulsion is then slowly sprayed on to the 190.6 g of tea (10% of bulk tea) using compressed air at a pressure of 4kg/cm2 and flow rate of 300ml/min in the Foerberg mixer for 12-15 min. The wet tea agglomerate thus made has approximately 15.47 % (theoretical) moisture content.
The wet tea agglomerate is dried in a Fluid bed drier for 10 min down to 2-3% moisture content. The 'flavour concentrate' thus made is diluted/blended with 1715.4g (1906g-190.6g) with 60g of Darjeeling Brokens in a vertical blender to get the final product.
Example 4: Using Composition-D of herbal flavours
For a batch size of 2 kg, the formulation details are mentioned in table 10.
Table 10. Details of formulation using Composition - D of herbal falvours
10g of encapsulant is added to the 25.77 ml of hot water with mixing using Silverson emulsifier for 5 min as described elsewhere, till a homogenous solution is formed. This solution is then allowed to cool to 50-60 °C followed by addition of all the flavour (total 11.18g) as mentioned in table 6. The resultant solution is then mixed again at 3000 rpm for 10 min to get an emulsion with 40% solids.
This emulsion is then slowly sprayed on to the 192.282 g of tea (10% of bulk tea) using compressed air at a pressure of 4kg/cm2 and flow rate 300ml/min in
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the Forberg mixer for 12-15 min. The wet tea agglomerate thus made has approximately 10.965 % (theoretical) moisture content.
The wet tea agglomerate is dried in a Fluid bed drier for 10 min down to 2-3% moisture content. The 'flavour concentrate' thus made is diluted/blended with 1730.538 (1922.82g-192.282g) with 60g of Darjeeling Brokens in a vertical blender to get the final product.
It is to be noted that the present invention is susceptible to modifications adaptations and changes by those skilled in the art, without departing from the scope of the present invention. Such modifications, adaptations, changes are intended to be within the scope of the present invention, which is further set forth under the claims that follow.
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We Claim:
1. A flavoured herbal tea composition comprising, as weight percentages of composition: 10-50% of flavour concentrate, 50-90% by weight of plain bulk tea, 1 to 8% by weight of Darjeeling Brokens, which is orthodox smaller or broken leaf grade of Darjeeling tea, wherein further flavour concentrate comprises 0.5 -5% by weight of natural herbal flavours, 0.3 to 0.7 % by weight of an encapsulant and rest as tea particles and wherein further said flavour concentrate is obtained by the steps of:
(a)preparing an emulsion by adding slowly 0.3 to 0.7% by weight of an encapsulant to hot water at temperature between 60°C and 80°C with mixing in an emulsifier for about 5 minutes till a homogenous solution is obtained; cooling the solution to 40-60°C; adding a combination of different natural herbal flavours selected from Composition-A, Composition-B, Composition-C and Composition-D as hereinafter described, so that the emulsion has a solid content in the range of 40 to 80% mixing the solution again at rotational speed higher than lOOOrpm for about 10 minutes, obtaining thereby an emulsion, wherein
- said composition-A of herbal flavours includes 0.1 - 0.5% of Bacopa monnierr, 0.3 - 0.7 % of Ocimum sanctum, 0.05 -0.3% of Mentha piperita, 0.05 - 0.3% of Zingiber officinalis and 0.1 - 0.3% of Elettaria cardamomum;
-said composition-B of herbal flavours includes 0.05 - 0.15% of Salvia officinalis, 0.5 - 0.11% of Glycyrrhiza glabra, 0.01 -0.09% of Mentha piperita and 0.1 - 0.3% of Zingiber officinalis ;
28
-said composition-C of herbal flavours includes 0.1 - 0.55% of Bacopa monnieri, 0.05 - 0.15% of Centella asiatica, 0.3 -0.7% of Ocimum sanctum, 0.1 - 0.3% of Zingiber officinalis, and 0.05 - 0.15% of Foeniculum vulgare; and
-said composition-D of herbal flavours includes 0.005 -0.013% of Trachispermum ammi, 0.1 - 0.2% of Mentha piperita, and 0.05 - 0.35% of Bettaria cardamomu;
(b) wet blending the tea particles with the emulsion as obtained by the
step (a) by spraying the said emulsion slowly on to the 10-50% of the
tea with mixing in a Foerberg mixer for 5 to 20, preferably 12 to 15
minutes for uniform coating thereby obtaining wet tea agglomerate of
tea particles with moisture content between 15 and 30% and
homogenously coated with the said emulsion; and
(c) drying the wet tea agglomerate obtained by step (b) above gently
but rapidly in a fluidized bed dryer with inlet air temperature of 70-
110°C preferably between 80-90°C and residence time of 6-10
minutes, till the moisture content is reduced to 2 to 3%, obtaining
thereby flavour concentrate.
2. A flavoured herbal tea composition as claimed in claim 1 said composition-
A includes natural herbal flavours 0.3% by weight of Bacopa monnieri,
0.5% by weight of Ocimum sanctum, 0.1% by weight of Mentha
piperita, 0.1% by weight of Zingiber officinalis and 0.5% by weight
of Elettaria cardamomum.
3. A flavoured herbal tea composition as claimed in claim 1 said composition-
B includes natural herbal flavours 0.1% by weight of Salvia officinalis,
29
0.8% by weight of Glycyrrhiza glabra, 0.05% by weight of Mentha piperita and 0.2% by weight of Zingiber officinalis.
4. A flavoured herbal tea composition as claimed in claim 1 said composition-
C includes natural herbal flavours 0.3% by weight of Bacopa monnieri,
0.1% by weight of Centella asiatica, 0.5% by weight of Ocimum
sanctum, 0.2% by weight of Zingiber officinalis and 0.1% by weight
of Foeniculum vulgare.
5. A flavoured herbal tea composition as claimed in claim 1 said composition-
D includes natural herbal flavours 0.009% by weight of Trachispermum
ammi, 0.15% by weight of Mentha piperita, and 0.2 % by weight of
Elettaria cardamomum.
6. A flavoured herbal tea composition as claimed in claim 1 wherein tea
includes black tea, green tea and oolong tea processed from leaf material
from Camellia sinensis van sinensis or Camellia sinensis van Assamica,
rooibos tea obtained from Aspalathus linearis, tea made by CTC or
orthodox methods and blends of two or more teas.
7. A flavoured herbal tea composition as claimed in claim 1 wherein said
emulsion has solids in the range of 50 to 70%.
8. A flavoured herbal tea composition as claimed in claim 1 wherein said
encapsulant is a modified starch derived from waxy maize.
9. A flavoured herbal tea composition as claimed in claim 1 wherein the
temperature of hot water used in the preparation of the said emulsion is
between 50 and 65°C.
30
10. A flavoured herbal tea composition as claimed in claim 1 wherein for the
preparation of said emulsion, liquid flavours(oils)/oleoresins may also be
optionally used, in addition to herbal flavours.
11. A flavoured herbal tea composition as claimed in claim 1 wherein the wet
tea agglomerate obtained after spraying the said emulsion has a moisture
content between 17 and 22%.
12. A flavoured herbal tea composition as claimed in claim 1 wherein said
Darjeeling Brokens comprise 2 to 4% by weight of composition.
13. A flavoured herbal tea composition as claimed in claim 1 wherein said
flavour concentrate included 1 to 1.5% by weight of herbal flavours.
14. A flavoured herbal tea composition as substantially described herein and
illustrated with examples and accompanying drawings.
15. A process for manufacturing flavoured herbal composition comprising the
steps of:
(a) Preparation of flavour concentrate by the steps of:
(i) preparing an emulsion by adding slowly 0.3 to 0.7% by weight of an encapsulant to hot water at temperature between 60°C and 80°C with mixing in an emulsifier for about 5 minutes till a homogenous solution is obtained; cooling the solution to 40-60°C; adding a combination of different natural herbal flavours selected from Composition-A, Composition-B, Composition-C and Composition-D as hereinafter described, so that the emulsion has a solid content in the range of 40 to 80% mixing the solution again at rotational speed
31
higher than 1000rpm for about 10 minutes, obtaining thereby an emulsion, wherein
-said composition-A of herbal flavours includes 0.1 - 0.5% of Bacopa monnieri, 0.3 - 0.7 % of Ocimum sanctum, 0.05 -0.3% of Mentha piperita, 0.05 - 0.3% of Zingiber officinalis and 0.1 - 0.3% of Elettaria cardamomum;
-said composition-B of herbal flavours includes 0.05 - 0.15% of Salvia officinalis, 0.5 - 0.11% of Glycyrrhiza glabra, 0.01 -0.09% of Mentha piperita and 0.1 - 0.3% of Zingiber officinalis ;
-said composition-C of herbal flavours includes 0.1 - 0.55% of Bacopa monnieri, 0.05 - 0.15% of Centella asiatica, 0.3 -0.7% of Ocimum sanctum, 0.1 - 0.3% of Zingiber officinalis, and 0.05 - 0.15% of Foeniculum vulgare; and
-said composition-D of herbal flavours includes 0.005 -0.013% of Trachispermum ammi, 0.1 - 0.2% of Mentha piperita, and 0.05 - 0.35% of Elettaria cardamomum;
(ii) wet blending the tea particles with the emulsion as obtained by the step (a) by spraying the said emulsion slowly on to the 10-50% of the tea with mixing in a Foerberg mixer for 5-20 minutes preferably 12-15 minutes for uniform coating obtaining thereby wet tea agglomerate of tea particles with moisture content between 15 and 30% and homogenously coated with the said emulsion; and
32
(iii) drying the wet tea agglomerate obtained by step (b) above gently but rapidly in a fluidized bed dryer with inlet air temperature of 70-110°C preferably between 80-90°C and residence time of 6-10 minutes, till the moisture content is reduced to 2 to 3%, obtaining thereby flavour concentrate.
(b) diluting/blending with 90 to 50% by weight of plain bulk tea and 1 to 8% of Darjeeling Brokens which is orthodox smaller or broken leaf grade of Darjeeling tea, to obtain the desired herbal flavoured tea composition
16. A process as claimed in claim 15 wherein said composition-A includes of
natural herbal flavours 0.3% by weight of Bacopa monnieri, 0.5% by
weight of Ocimum sanctum, 0.1% by weight of Mentha piperita,
0.1% by weight of Zingiher officinalis and 0.5% by weight of
Elettaria cardamomum.
17. A process as claimed in claim 15 wherein said composition-B includes
natural herbal flavours 0.1% by weight of Salvia officinalis, 0.8% by
weight of Glycyrrhiza glabra, 0.05% by weight of Mentha piperita
and 0.2% by weight of Zingiber officinalis.
18. A process as claimed in claim 15 wherein said composition-C includes of
natural herbal flavours 0.3% by weight of Bacopa monnieri, 0.1% by
weight of Centella asiatica, 0.5% by weight of Ocimum sanctum,
0.2% by weight of Zingiber officinalis and 0.1% by weight of
Foeniculum vulgare.
19. A process as claimed in claim 15 wherein Composition-D includes natural
herbal flavours 0.009% by weight of Trachispermum ammi, 0.15% by
weight of Mentha piperita, and 0.2 % by weight of Elettaria
cardamomum.
33
20. A flavoured herbal tea composition as claimed in claim 15 wherein said
emulsion has solids in the range of 50 to 70%.
21. A process as claimed in claim 15 wherein said encapsulant is a modified
starch derived from waxy maize.
22. A flavoured herbal tea composition as claimed in claim 15 wherein the
temperature of hot water used in the preparation of the said emulsion is
between 50 and 65°C.
23. A flavoured herbal tea composition as claimed in claim 15 wherein tea
includes black tea, green tea and oolong tea processed from leaf material
from Camellia sinensis var. sinensis or Camellia sinensis var. Assamica,
rooibos tea obtained from Aspalathus linearis, tea made by CTC or
orthodox methods and blends of two or more teas.
24. A flavoured herbal tea composition as claimed in claim 15 wherein for the
preparation of said emulsion, liquid flavours(oils)/oleoresins may also be
optionally used, in addition to herbal flavours.
25. A flavoured herbal tea composition as claimed in claim 15 wherein the wet
tea agglomerate obtained after spraying the said emulsion has moisture
content between 17 and 22%.
26. A flavoured herbal tea composition as claimed in claim 15 wherein said
Darjeeling Brokens comprise 2 to 4% by weight of composition
27. A flavoured herbal tea composition as claimed in claim 15 wherein said
flavour concentrate included 1 to 1.5% by weight of herbal flavours.
34
28. A process for preparation of flavoured herbal tea composition as substantially described and illustrated with examples and accompanying drawings.
The present invention relates to an herbal flavoured tea composition and a process for its manufacturing. The process of manufacture provides four variant compositions of herbal flavoured tea by using four combinations of herbal flavours. The combinations of herbal flavours include herbs like Bacopa monnieri, Ocimum sanctum, Mentha piperita etc. The process involves blending of flavour concentrate with Darjeeling Brokens and plain bulk tea. The flavour concentrate is made by preparing an emulsion by adding an encapsulant in water, adding natural flavours, spraying the emulsion of natural flavours onto 10-50% of the tea used in formulation followed by gentle and rapid drying in a fluidised bed drier. The herbal flavoured tea composition manufactured by the process has unique texture, taste like tea and has higher shelf life stability. The modification of the final taste of the final tea product can be achieved by adjustment during the dilution/ blending stage.
| Section | Controller | Decision Date |
|---|---|---|
| 15 | Dr. Sukanya Chattopadhyay | 2015-11-05 |
| 25(1) to read with 55 | Dr. Sukanya Chattopadhyay | 2015-11-05 |
| # | Name | Date |
|---|---|---|
| 1 | 359-KOL-2007-(31-12-2010)-FORM-13.pdf | 2010-12-31 |
| 1 | 359-KOL-2007_EXAMREPORT.pdf | 2016-06-30 |
| 2 | 359-KOL-2007-(09-09-2011)-CORRESPONDENCE.pdf | 2011-09-09 |
| 2 | Request For Certified Copy-Online.pdf | 2016-01-19 |
| 3 | REQUEST FOR CERTIFIED COPY [18-01-2016(online)].pdf | 2016-01-18 |
| 3 | 359-KOL-2007-PRE GRANT OPPOSITION.pdf | 2011-10-06 |
| 4 | 359-KOL-2007-PA.pdf | 2011-10-06 |
| 4 | 359-KOL-2007-(27-10-2015)-AMENDED PAGES.pdf | 2015-10-27 |
| 5 | 359-KOL-2007-OTHERS.pdf | 2011-10-06 |
| 5 | 359-KOL-2007-(27-10-2015)-CLAIMS.pdf | 2015-10-27 |
| 6 | 359-KOL-2007-FORM 2.1.1.pdf | 2011-10-06 |
| 6 | 359-KOL-2007-(27-10-2015)-COPY OF FORM-13.pdf | 2015-10-27 |
| 7 | 359-KOL-2007-FORM 13.pdf | 2011-10-06 |
| 7 | 359-KOL-2007-(27-10-2015)-CORRESPONDENCE.pdf | 2015-10-27 |
| 8 | 359-KOL-2007-FORM 13.1.1.pdf | 2011-10-06 |
| 8 | 359-KOL-2007-(27-10-2015)-DESCRIPTION (COMPLETE).pdf | 2015-10-27 |
| 9 | 359-KOL-2007-(27-10-2015)-FORM-2.pdf | 2015-10-27 |
| 9 | 359-KOL-2007-DESCRIPTION (COMPLETE) 1.1.pdf | 2011-10-06 |
| 10 | 359-KOL-2007-(27-10-2015)-MARKEDUP CLAIMS.pdf | 2015-10-27 |
| 10 | 359-KOL-2007-CORRESPONDENCE-1.6.pdf | 2011-10-06 |
| 11 | 359-KOL-2007-(27-10-2015)-MARKEDUP FORM-2.pdf | 2015-10-27 |
| 11 | 359-KOL-2007-CORRESPONDENCE-1.5.pdf | 2011-10-06 |
| 12 | 359-KOL-2007-(24-09-2015)-CORRESPONDENCE.pdf | 2015-09-24 |
| 12 | 359-KOL-2007-CORRESPONDENCE-1.2.pdf | 2011-10-06 |
| 13 | 359-KOL-2007-(24-09-2015)-HEARING ON PREGRANT OPPOSITION.pdf | 2015-09-24 |
| 13 | 359-KOL-2007-CORRESPONDENCE 1.8.pdf | 2011-10-06 |
| 14 | 359-KOL-2007-(24-09-2015)-OTHERS.pdf | 2015-09-24 |
| 14 | 359-KOL-2007-CORRESPONDENCE 1.7.pdf | 2011-10-06 |
| 15 | 359-KOL-2007-(16-09-2015)-OPPOSITION UNDER SECTION(25).pdf | 2015-09-16 |
| 15 | 359-KOL-2007-CORRESPONDENCE 1.4.pdf | 2011-10-06 |
| 16 | 359-KOL-2007-(16-09-2015)-PREGRANT HEARING SUBMISSION-(ADVANCE COPY).pdf | 2015-09-16 |
| 16 | 359-KOL-2007-CORRESPONDENCE 1.3.pdf | 2011-10-06 |
| 17 | 359-KOL-2007-CORRESPONDENCE 1.1.pdf | 2011-10-06 |
| 17 | 359-KOL-2007-(10-09-2015)-CORRESPONDENCE.pdf | 2015-09-10 |
| 18 | 359-KOL-2007-(11-05-2012)-CORRESPONDENCE.pdf | 2012-05-11 |
| 18 | 359-KOL-2007-AMANDED CLAIMS.pdf | 2011-10-06 |
| 19 | 00359-kol-2007 correspondence-1.1.pdf | 2011-10-06 |
| 19 | 359-KOL-2007-ABSTRACT 1.1.pdf | 2011-10-06 |
| 20 | 00359-kol-2007 form-18.pdf | 2011-10-06 |
| 20 | 0359-kol-2007 form-3.pdf | 2011-10-06 |
| 21 | 00359-kol-2007-assignment.pdf | 2011-10-06 |
| 21 | 0359-kol-2007 form-2.pdf | 2011-10-06 |
| 22 | 00359-kol-2007-correspondence-1.2.pdf | 2011-10-06 |
| 22 | 0359-kol-2007 form-1.pdf | 2011-10-06 |
| 23 | 00359-kol-2007-correspondence-1.3.pdf | 2011-10-06 |
| 23 | 0359-kol-2007 drawings.pdf | 2011-10-06 |
| 24 | 0359-kol-2007 description(complete).pdf | 2011-10-06 |
| 24 | 00359-kol-2007-correspondence.pdf | 2011-10-06 |
| 25 | 00359-kol-2007-form-1-1.1.pdf | 2011-10-06 |
| 25 | 0359-kol-2007 correspondence others.pdf | 2011-10-06 |
| 26 | 00359-kol-2007-form-9.pdf | 2011-10-06 |
| 26 | 0359-kol-2007 claims.pdf | 2011-10-06 |
| 27 | 00359-kol-2007-g.p.a.pdf | 2011-10-06 |
| 27 | 0359-kol-2007 abstract.pdf | 2011-10-06 |
| 28 | 00359-kol-2007-g.p.a.pdf | 2011-10-06 |
| 28 | 0359-kol-2007 abstract.pdf | 2011-10-06 |
| 29 | 00359-kol-2007-form-9.pdf | 2011-10-06 |
| 29 | 0359-kol-2007 claims.pdf | 2011-10-06 |
| 30 | 00359-kol-2007-form-1-1.1.pdf | 2011-10-06 |
| 30 | 0359-kol-2007 correspondence others.pdf | 2011-10-06 |
| 31 | 00359-kol-2007-correspondence.pdf | 2011-10-06 |
| 31 | 0359-kol-2007 description(complete).pdf | 2011-10-06 |
| 32 | 00359-kol-2007-correspondence-1.3.pdf | 2011-10-06 |
| 32 | 0359-kol-2007 drawings.pdf | 2011-10-06 |
| 33 | 00359-kol-2007-correspondence-1.2.pdf | 2011-10-06 |
| 33 | 0359-kol-2007 form-1.pdf | 2011-10-06 |
| 34 | 00359-kol-2007-assignment.pdf | 2011-10-06 |
| 34 | 0359-kol-2007 form-2.pdf | 2011-10-06 |
| 35 | 00359-kol-2007 form-18.pdf | 2011-10-06 |
| 35 | 0359-kol-2007 form-3.pdf | 2011-10-06 |
| 36 | 359-KOL-2007-ABSTRACT 1.1.pdf | 2011-10-06 |
| 36 | 00359-kol-2007 correspondence-1.1.pdf | 2011-10-06 |
| 37 | 359-KOL-2007-(11-05-2012)-CORRESPONDENCE.pdf | 2012-05-11 |
| 37 | 359-KOL-2007-AMANDED CLAIMS.pdf | 2011-10-06 |
| 38 | 359-KOL-2007-(10-09-2015)-CORRESPONDENCE.pdf | 2015-09-10 |
| 38 | 359-KOL-2007-CORRESPONDENCE 1.1.pdf | 2011-10-06 |
| 39 | 359-KOL-2007-(16-09-2015)-PREGRANT HEARING SUBMISSION-(ADVANCE COPY).pdf | 2015-09-16 |
| 39 | 359-KOL-2007-CORRESPONDENCE 1.3.pdf | 2011-10-06 |
| 40 | 359-KOL-2007-(16-09-2015)-OPPOSITION UNDER SECTION(25).pdf | 2015-09-16 |
| 40 | 359-KOL-2007-CORRESPONDENCE 1.4.pdf | 2011-10-06 |
| 41 | 359-KOL-2007-(24-09-2015)-OTHERS.pdf | 2015-09-24 |
| 41 | 359-KOL-2007-CORRESPONDENCE 1.7.pdf | 2011-10-06 |
| 42 | 359-KOL-2007-(24-09-2015)-HEARING ON PREGRANT OPPOSITION.pdf | 2015-09-24 |
| 42 | 359-KOL-2007-CORRESPONDENCE 1.8.pdf | 2011-10-06 |
| 43 | 359-KOL-2007-(24-09-2015)-CORRESPONDENCE.pdf | 2015-09-24 |
| 43 | 359-KOL-2007-CORRESPONDENCE-1.2.pdf | 2011-10-06 |
| 44 | 359-KOL-2007-(27-10-2015)-MARKEDUP FORM-2.pdf | 2015-10-27 |
| 44 | 359-KOL-2007-CORRESPONDENCE-1.5.pdf | 2011-10-06 |
| 45 | 359-KOL-2007-(27-10-2015)-MARKEDUP CLAIMS.pdf | 2015-10-27 |
| 45 | 359-KOL-2007-CORRESPONDENCE-1.6.pdf | 2011-10-06 |
| 46 | 359-KOL-2007-DESCRIPTION (COMPLETE) 1.1.pdf | 2011-10-06 |
| 46 | 359-KOL-2007-(27-10-2015)-FORM-2.pdf | 2015-10-27 |
| 47 | 359-KOL-2007-FORM 13.1.1.pdf | 2011-10-06 |
| 47 | 359-KOL-2007-(27-10-2015)-DESCRIPTION (COMPLETE).pdf | 2015-10-27 |
| 48 | 359-KOL-2007-FORM 13.pdf | 2011-10-06 |
| 48 | 359-KOL-2007-(27-10-2015)-CORRESPONDENCE.pdf | 2015-10-27 |
| 49 | 359-KOL-2007-FORM 2.1.1.pdf | 2011-10-06 |
| 49 | 359-KOL-2007-(27-10-2015)-COPY OF FORM-13.pdf | 2015-10-27 |
| 50 | 359-KOL-2007-OTHERS.pdf | 2011-10-06 |
| 50 | 359-KOL-2007-(27-10-2015)-CLAIMS.pdf | 2015-10-27 |
| 51 | 359-KOL-2007-(27-10-2015)-AMENDED PAGES.pdf | 2015-10-27 |
| 51 | 359-KOL-2007-PA.pdf | 2011-10-06 |
| 52 | 359-KOL-2007-PRE GRANT OPPOSITION.pdf | 2011-10-06 |
| 52 | REQUEST FOR CERTIFIED COPY [18-01-2016(online)].pdf | 2016-01-18 |
| 53 | 359-KOL-2007-(09-09-2011)-CORRESPONDENCE.pdf | 2011-09-09 |
| 53 | Request For Certified Copy-Online.pdf | 2016-01-19 |
| 54 | 359-KOL-2007-(31-12-2010)-FORM-13.pdf | 2010-12-31 |
| 54 | 359-KOL-2007_EXAMREPORT.pdf | 2016-06-30 |