Claims:WE CLAIM:
1. A method for preparing a composition in which adulteration can be detected, said method comprising blending a fluorophore therein in an amount in the range of 0.0005 wt% to 0.5 wt%, to enable the content of fluorophore to be detected such that adulteration of said composition and the extent of adulteration is determined.
2. The method as claimed in claim 1, wherein the average particle size of said fluorophore in said composition is in the range of 1 µm to 10 µm.
3. The method as claimed in claim 1, wherein said fluorophore is selected from the group consisting of thiophene derivatives, oxazine derivatives, and quinazolinone derivatives.
4. The method as claimed in claim 1, wherein said fluorophore is (2,5-Di(5-tert-butylbenzoxazol-2-yl)thiophene).
5. A composition having a fluorophore in an amount in the range of 0.0005 wt% to 0.5 wt%, wherein the content of said fluorophore is detected such that adulteration of said composition and the extent of adulteration are determined.
6. The method as claimed in claim 5, wherein said composition is selected from paint composition, adhesive composition, ink composition, and cosmetic composition.
7. The method as claimed in claim 5, wherein the form of said composition is selected from wet form, dry form, and film form.
8. The method as claimed in claim 7, wherein said film has a dry film thickness (DFT) of 0.01 mm and above.
9. The method as claimed in claim 7, wherein said film has a dry film thickness (DFT) in the range of 0.01 mm to 10 mm.
10. A method for detecting adulteration in a composition as claimed in claim 1, said method comprising the following steps:
a. obtaining a composition comprising a fluorophore;
b. externally adding a solvent capable of extracting said fluorophore from said composition under stirring to obtain a biphasic mixture having a solvent layer comprising said fluorophore and a resultant layer;
c. separating said solvent layer comprising said fluorophore from said biphasic mixture;
d. detecting the presence of said fluorophore in said solvent layer under UV source; and
e. analyzing the change in the intensity of said fluorophore under said UV source in said solvent layer to detect the extent of adulteration in said composition.
11. The method as claimed in claim 10, wherein said change in intensity of said fluorophore in said solvent layer is detected by observing the change in visual appearance of said solvent layer.
12. The method as claimed in claim 10, wherein said change in intensity of said fluorophore in said solvent layer is detected by measuring the intensity of the emission at a wavelength in the range of 400 nm to 700 nm.
13. The method as claimed in claim 10, wherein said solvent is selected from the group consisting of an alcohol, ketone, ether, an ester, and a hydrocarbon.
14. The method as claimed in claim 10, wherein said solvent is selected from the group consisting of glycol, cyclohexanone, xylene, iso butanol, carbon tetrachloride and chloroform.
, Description:FIELD
The present disclosure relates to a method for preparing a composition and a method for detecting adulteration in a composition.
DEFINITIONS
As used in the present disclosure, the following terms are generally intended to have the meaning as set forth below, except to the extent that the context in which they are used indicate otherwise.
The term “adulteration” as used herein refers to the presence of an undesirable substance within another substance, such as food, fuel, or chemicals or replacement of an original substance with another substance.
The term “fluorophore”, also known as taggant, as used herein refers to a fluorescent chemical compound that can re-emit light upon UV excitation. Fluorophores, typically contain several combined aromatic groups, or planar or cyclic molecules with several p bonds.
The term “Hegman gauge” as used herein refers to a device used to determine the fineness of the ground particles of pigment (or other solid) dispersed in a sample of paint (or other liquid).
BACKGROUND
The background information herein below relates to the present disclosure but is not necessarily prior art.
High-value proprietary products are often copied and offered for sale in remarkably convincing packaging in spite of being protected. The well-equipped and highly skilled individuals are able to copy many important products and are placed in the market, illegally. The imitation or copying of the product does not only harm the market of the original product, but also gives rise to fears of considerable health damage/risk to the consumers. Therefore, the protection of products against imitation and counterfeiting is important.
Dealing with such issues, is not only concerned with the prevention of the falsifying, illegal copying or all kinds of faking, but also with the methods for proper identification and a provision that will allow identifying the originality/ authenticity of the product.
Therefore, there is felt a need for a method for preparing a composition and a method for detecting adulteration in a composition.
OBJECTS
Some of the objects of the present disclosure, which at least one embodiment herein satisfies, are as follows:
It is an object of the present disclosure to ameliorate one or more problems of the prior art or to at least provide a useful alternative.
Another object of the present disclosure is to provide a method for preparing a composition.
Yet another object of the present disclosure is to provide a method for detecting adulteration in a composition.
Still another object of the present disclosure is to provide a simple, accurate, rapid, and efficient method for detecting adulteration in a composition.
Other objects and advantages of the present disclosure will be more apparent from the following description, which is not intended to limit the scope of the present disclosure.

SUMMARY
The present disclosure relates to a method for preparing a composition in which adulteration can be detected. The method comprises blending a fluorophore into the composition in an amount in the range of 0.005 wt% to 0.5 wt%, to enable the content of fluorophore to be detected such that adulteration of the composition and the extent of adulteration can be determined.
The present disclosure further provides a composition having a fluorophore. The composition comprises a fluorophore in an amount in the range of 0.0005 wt% to 0.5 wt%, such that adulteration and extent of adulteration of the composition can be determined.
The present disclosure also provides a method for detecting adulteration in a composition. The method comprises obtaining a composition comprising a fluorophore. A solvent capable of extracting the fluorophore from the composition is externally added to the composition under stirring to obtain a biphasic mixture having a solvent layer comprising the fluorophore and a resultant layer. The solvent layer comprising the fluorophore is separated from the biphasic mixture. The fluorophore in the solvent layer can be detected under UV source. The change in the intensity of the fluorophore under the UV source, in the solvent layer is analyzed to determine the extent of adulteration in the composition. In one embodiment, the change in intensity of the fluorophore in the solvent layer is detected by observing the change in visual appearance of the solvent layer. In another embodiment, the change in intensity of the fluorophore in the solvent layer is detected by measuring the intensity of the emission at a wavelength in the range of 400 nm to 700 nm.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING
The process of the present disclosure will now be described with the help of the accompanying drawing, in which:
Figure 1a illustrates the comparison of solvent layer from an unadulterated composition (original composition) with adulterated compositions based on visual appearance in daylight in accordance with an embodiment of the present disclosure;
Figure 1b illustrates the comparison solvent layer from an unadulterated composition (original composition) with adulterated compositions based on intensity of the emission under UV exposure in accordance with an embodiment of the present disclosure;
Figure 2a illustrates a spectral image of a composition comprising organic yellow pigment and a fluorophore in the absence of a solvent;
Figure 2b illustrates a spectral image of a composition comprising organic yellow pigment and a fluorophore exhibiting blue emission extracted in a solvent (iso butanol);
Figure 3a illustrates a spectral image of a composition comprising organic yellow pigment and a fluorophore exhibiting green emission in the presence of a solvent; and
Figure 3b illustrates a spectral image of a composition comprising organic yellow pigment and a fluorophore exhibiting yellow emission extracted in a solvent (carbon tetrachloride).
DETAILED DESCRIPTION
Embodiments, of the present disclosure, will now be described with reference to the accompanying drawing.
Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, known processes or well-known apparatus or structures, and well known techniques are not described in detail.
The terminology used, in the present disclosure, is only for the purpose of explaining a particular embodiment and such terminology shall not be considered to limit the scope of the present disclosure. As used in the present disclosure, the forms "a,” "an," and "the" may be intended to include the plural forms as well, unless the context clearly suggests otherwise. The terms "comprises," "comprising," “including,” and “having,” are open ended transitional phrases and therefore specify the presence of stated features, integers, steps, operations, elements, modules, units and/or components, but do not forbid the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. The particular order of steps disclosed in the method and process of the present disclosure are not to be construed as necessarily requiring their performance as described or illustrated. It is also to be understood that additional or alternative steps may be employed.
The terms first, second, third, etc., should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer or section. Terms such as first, second, third, etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
In an aspect of the present disclosure, there is provided a method for preparing a composition in which adulteration can be detected. The method comprises blending a fluorophore therein in an amount in the range of 0.0005 wt% to 0.5 wt%, to enable the content of fluorophore to be detected such that adulteration of the composition and the extent of adulteration can be determined.
In accordance with the embodiments of the present disclosure, the average particle size of the fluorophore in the composition can be in the range of 1 µm to 10 µm. The fluorophore can be selected from the group consisting of thiophene derivatives, oxazine derivatives, and quinazolinone derivatives. In an embodiment, the fluorophore is (2, 5-Di (5-tert-butylbenzoxazol-2-yl) thiophene).
In another aspect of the present disclosure, there is provided a composition. The composition comprises a fluorophore in an amount in the range of 0.0005 wt% to 0.5 wt%. The content of the fluorophore is detected, such that adulteration of the composition and the extent of adulteration are determined.
The composition can be selected from paint composition, coating composition, adhesive composition, ink composition, cosmetic composition such as nail paints, body lotions, creams, and the like. In an embodiment the composition is paint composition selected from water and solvent borne paints, putties, powder coatings, adhesives, industrial coatings, wood coatings and floor coatings comprising fluorophore which exhibit emission under UV radiation.
The composition can be in the form of wet composition, dry composition, and film. In an embodiment, the composition is wet composition. In another embodiment, the composition is dry composition. In yet another embodiment, the composition is in the form of film.
The film can be dry film or wet film. In an embodiment, the film is dry film. In another embodiment, the dry film has a dry film thickness of 0.01 mm and above. In one embodiment the dry film thickness is in the range of 0.01 mm to 10 mm.
The present disclosure in a further aspect provides a method for detecting adulteration in a composition.
The method comprises obtaining a composition comprising a fluorophore.
Typically, the average particle size of the fluorophore in the composition can be in the range of 1 µm to 10 µm. The fluorophore is at least one selected from the group consisting of thiophene derivatives, oxazine derivatives, and quinazolinone derivatives. In an embodiment, the fluorophore is (2,5-Di(5-tert-butylbenzoxazol-2-yl)thiophene).
A solvent is externally added to the composition (the composition is suspected to be adulterated) under stirring to obtain a biphasic mixture having a solvent layer comprising the fluorophore and a resultant layer. The solvent used in the method is capable of extracting the fluorophore from the composition.
Typically, the solvent in an amount of 1 to 2 ml is capable of extracting the fluorophore if present in the composition. However, the fluorophore can be also extracted, if higher amount of solvent is used.
Typically, the solvent can be polar or non-polar, and can be selected from the group consisting of an alcohol, ketone, ether, an ester, and a hydrocarbon. In an embodiment the solvent can be selected from glycol, cyclohexanone, xylene, iso butanol, carbon tetrachloride, and chloroform. In an embodiment, the solvent is iso butanol. In another embodiment, the solvent is carbon tetrachloride.
Further, the solvent layer comprising the fluorophore is separated from the biphasic mixture
In accordance with an embodiment of the present disclosure, the solvent layers separated from standard and samples adulterated with different percentages of spurious colorants as viewed under day light is illustrated in Figure 1a. It is seen from Figure 1a that, there is very little visual difference between the solvent layer separated from the standard and the ones separated from the adulterated samples.
Figure 1b depicts the solvent layers separated from standard and samples adulterated with different percentages of spurious colorants as viewed under a UV source. It is clearly evident that the fluorophore in the solvent layer can be detected under a UV source.

The change in the intensity of the fluorophore under the UV source, in the solvent layer is then analyzed to determine the extent of adulteration in the composition.
In one embodiment, the change in intensity of the fluorophore in the solvent layer is detected by observing the change in visual appearance of the solvent layer as illustrated in Figure-1b.
In another embodiment, the change in intensity of the fluorophore in the solvent layer is detected by measuring the intensity of the emission at a wavelength in the range of 400 nm to 700 nm as illustrated in Figure-2b. Though, the excitation of the fluorophore takes place under UV radiations, the emission occurs in the visible light.
In accordance with the present disclosure, it is observed that the emission under the UV radiation is not observed if the amount of the fluorophore is below 0.0005%. The addition of specific solvent makes it possible for the fluorophore to emit a characteristic emission (GLOW).
In accordance with the present disclosure, the amount of the fluorophore in the composition is typically in the range of 0.0005 wt% to 0.5 wt%.
In an embodiment, if the amount of fluorophore in a composition is below 0.007%, emission under UV radiation is not exhibited, however, the characteristic emission can be observed by the addition of suitable solvent. The solvent extracts fluorophore from the composition and the solvent comprising fluorophore exhibits emission (fluorescence). The selection of the solvent for a particular fluorophore is an important aspect in accordance with the present disclosure.
In an embodiment, the authenticity of a composition in wet form is determined by taking 0.1ml to 5ml composition on a glass plate/a petri dish or in a tin container lid and adding few drops of suitable solvent. The composition exhibits characteristic glow (fluorescence) under source of UV radiation.
In another embodiment, the authenticity of a composition in film form having a thickness in the range from 0.01 mm to 1 mm is determined by adding a suitable solvent to the dried film of the composition containing fluorophore. Characteristic fluorescence is observed on exposure to UV radiations, such as 365 nm.
It is possible using the method of present disclosure to achieve the characteristic UV fluorescence by addition of the suitable solvent in compositions comprising fluorophore in a pigmented system, wherein pigment absorbs UV radiation and does not allow fluorophore to glow under UV light.
In one embodiment of the present disclosure, fluorophore can be incorporated in different water borne, solvent borne and powder products. Fluorophore is externally added in finished products like paints, putties, powder coatings, adhesives, industrial coatings, wood coatings and floor coatings and the tagged materials exhibit glow under UV radiation. Same study is carried out on a dry film of above products on different surfaces like wood, metal and masonry surfaces. In pigmented systems suitable organic solvent is needed to identify authentic product containing fluorophore.
Viscosity, density and other physical parameter remain unaffected due to very optimum amount of fluorophore added in the formulation. If the fluorophore in the formulation is below 0.007%, fluorescence under UV radiation source is not exhibited, whereas addition of suitable polar/non-polar solvent extracts the fluorophore particles on the surface of the colorant/paint and high intensity fluorescence is exhibited. No adverse effect on colorant/paint or degradation of fluorescence intensity is observed. In an embodiment organic yellow with different amount of fluorophore, organic orange, organic magenta, inorganic yellow, inorganic black, interior acrylic paint, and exterior acrylic paint is used. Average particle size of fluorophore is about 1 – 10 µm which does not affect Hegman gauge finish of colorant/paint.
The method of the present disclosure is able to identify authentic products adulterated by clones with the help of suitable organic solvent. It is very valuable to use fluorophore in various organic and inorganic pigments having different UV absorption and emission phenomena. A fixed amount of fluorophore exhibits a different UV absorption and emission phenomena in various organic or inorganic pigment formulation which hampers detection technique methodology. Fluorophore present in the product is extracted with the help of suitable organic solvent when an organic solvent is mixed with the product. The supernatant organic solvent containing fluorophore can be separated out and taken in a glass tube. The concentration of fluorophore in the product gets diluted if adulterated with clone and the intensity of glow of fluorophore in a fixed amount of suitable solvent decreases under UV source. If the entire original composition is replaced by a spurious composition the same can be detected by merely adding the solvent, followed by exposure to UV radiation. A spurious sample does not exhibit fluorescence whereas the original sample on visual evaluation exhibits fluorescence.
The composition of the present disclosure retains the fluorescence even on exposure to external weathering.
The foregoing description of the embodiments has been provided for purposes of illustration and not intended to limit the scope of the present disclosure. Individual components of a particular embodiment are generally not limited to that particular embodiment, but, are interchangeable. Such variations are not to be regarded as a departure from the present disclosure, and all such modifications are considered to be within the scope of the present disclosure.
The present disclosure is further described in light of the following experiments which are set forth for illustration purpose only and not to be construed for limiting the scope of the disclosure. The following experiments can be scaled up to industrial/commercial scale and the results obtained can be extrapolated to industrial scale.

EXPERIMENTAL DETAILS:
General procedure for preparation of Colorant
In a stainless steel vessel 35 – 50% Water, 10 – 25% Wetting and Dispersing Agent, 10 – 20% Glycol, 0 – 2% Preservative, 0 – 5% pH stabilizer and 0 – 5% Defoamer were added. This mixture was stirred for 5 minutes by using Impeller disk stirrer. 10 – 30% Organic Pigment, 0 – 10% Extender and 0.003 – 0.007% Fluorophore having average particle size of about 1 – 10 µm was added. This Mixture was ground with the help of grinding media of size 0.5 – 3 mm for approx. 30 mins. Formulation was thinned to 100% with the help of Glycol, Surfactant, Preservative, Defoamer, and Water.
The extent of adulteration was quantified using LR1 – compact fluorescence spectroscopy instrument (ASEQ Instruments). An enclosed UV chamber containing 365 nm and 9 watt UV source was used to activate emission of the fluorophore. Portable UV torch of 365nm and 3 watt can also provide the desired performance.
Experiment-1: (Organic Magenta + 0.005% Fluorophore)
2 ml of a (organic Magenta colorant) having 0.005 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed. The colorant comprising fluorophore cannot be distinguished visually from colorant without fluorophore.
2-4 drops of Iso-butanol were added on the colorant surface. Blue fluorescence was observed.
Experiment 2: (Organic Orange + 0.005% Fluorophore)
2 ml of a (organic Orange colorant) having 0.005 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The colorant comprising fluorophore cannot be distinguished visually from colorant without fluorophore.
2-4 drops of Iso-butanol were added on the colorant surface. Blue fluorescence was observed.
Experiment 3: (Organic Yellow + 0.005% Fluorophore)
2 ml of a (organic Yellow colorant) having 0.005 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The colorant comprising fluorophore cannot be distinguished visually from colorant without fluorophore.
Figure-2a illustrates the spectral graph of the formulation with fluorophore without solvent. Figure-2b illustrates the spectral graph of a formulation with fluorophore and 2-4 drops of Isobutanol. It is clearly seen that the blue fluorescence is only observed in the presence of isobutanol
Experiment 4: (Inorganic Yellow Oxide + 0.005% Fluorophore)
2 ml of a (inorganic Yellow colorant) having 0.005 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV light source. The colorant comprising fluorophore cannot be distinguished visually from colorant without fluorophore.
2-4 drops of isobutanol were added on the colorant surface. Blue fluorescence was observed.
Experiment 5: (Organic Yellow + 0.5% Green Fluorophore)
2 ml of an organic Yellow colorant having 0.5 % of green fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The colorant comprising fluorophore cannot be distinguished visually from colorant without fluorophore.
2-4 drops of Carbon tetrachloride were added on the colorant surface. Green fluorescence was observed spectrally as illustrated in Figure-3a.

Experiment 6: (Organic Yellow + 0.5% Yellow Fluorophore)
2 ml of an organic Yellow colorant having 0.5 % of yellow fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The colorant comprising fluorophore cannot be distinguished visually or spectrally from colorant without fluorophore.
2-4 drops of Carbon tetrachloride were added on the colorant surface. Yellow fluorescence was observed spectrally as illustrated in Figure-3b.
Experiment 7: (Exterior Acrylic Paint + 0.001% Fluorophore)
2 ml of an exterior Acrylic Paint having 0.001 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The exterior paint comprising fluorophore cannot be distinguished visually from exterior paint without fluorophore.
2-4 drops of Iso-butanol were added on the paint surface. Blue fluorescence was observed.
Experiment 8: (Exterior Acrylic Paint + 0.005% Fluorophore)
2 ml of an Exterior Acrylic Paint having 0.005 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The exterior paint comprising fluorophore cannot be distinguished visually from exterior paint without fluorophore.
2-4 drops of Iso-butanol were added on the paint surface. Blue fluorescence was observed.
Experiment 9: (Interior Acrylic Paint + 0.005% Fluorophore)
2 ml of an Interior Acrylic Paint having 0.005 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The interior paint comprising fluorophore cannot be distinguished visually from interior paint without fluorophore.
2-4 drops of Iso-butanol were added on the paint surface. Blue fluorescence was observed.
Experiment 10: (Inorganic Black + 0.005% Fluorophore)
2 ml of an Inorganic Black colorant having 0.005 % of blue fluorophore was taken on a glass plate and kept under UV. No fluorescence was observed under UV source. The colorant comprising fluorophore cannot be distinguished visually from colorant without fluorophore.
2-4 drops of Iso-butanol were added on the colorant surface. Blue fluorescence was observed.
Experiment-11: Method for determining adulteration in a composition using visible light (visual appearance) in accordance with an embodiment of the present disclosure
2ml colorant containing the fluorophore was poured in to a petri-dish and 1 ml of solvent was added. Emission of characteristic light of the fluorophore is observed visually.
All above formulations are in accordance with the present disclosure, it was found that the colorant and base formulations were stable and UV glow of incorporated fluorophore remains unaffected even if the material is exposed to 55°C temperature for 1 month. None of the physical or chemical property of paint was affected after incorporation of above mentioned fluorophore. It was also found by way of the present invention that average particle size of 1 – 10 µm do not affect the finish of paint or colorant which is a primary requirement.
It is thus possible by way of the present advancement to provide for colorant and base formulations which did not show UV glow. High intensity UV glow is selectively achieved by way of the present invention by addition of polar, partially polar, and nonpolar organic solvents in selective amount to extract fluorophore from colorant or base surfaces and enhance UV glow intensity.
TECHNICAL ADVANCEMENTS
The present disclosure described herein above has several technical advantages including, but not limited to, the realization of a method for detecting adulteration of a composition that the method is simple, accurate, rapid, and efficient.
Throughout this specification the word “comprise”, or variations such as “comprises” or “comprising”, will be understood to imply the inclusion of a stated element, integer or step, or group of elements, integers or steps, but not the exclusion of any other element, integer or step, or group of elements, integers or steps.
The use of the expression “at least” or “at least one” or “a” suggests the use of one or more elements or ingredients or quantities, as the use may be in the embodiment of the invention to achieve one or more of the desired objects or results. While certain embodiments of the inventions have been described, these embodiments have been presented by way of example only, and are not intended to limit the scope of the inventions. Variations or modifications to the formulation of this invention, within the scope of the invention, may occur to those skilled in the art upon reviewing the disclosure herein. Such variations or modifications are well within the spirit of this invention.
The numerical values given for various physical parameters, dimensions, and quantities are only approximate values and it is envisaged that the values higher than the numerical value assigned to the physical parameters, dimensions and quantities fall within the scope of the invention unless there is a statement in the specification to the contrary.
While considerable emphasis has been placed herein on the specific features of the preferred embodiment, it will be appreciated that many additional features can be added and that many changes can be made in the preferred embodiment without departing from the principles of the disclosure. These and other changes in the preferred embodiment of the disclosure will be apparent to those skilled in the art from the disclosure herein, whereby it is to be distinctly understood that the foregoing descriptive matter is to be interpreted merely as illustrative of the disclosure and not as a limitation.