Description:Technical field of the invention:
The present invention relates to improved hair care products to reduce hair fall and increase hair strength and hair growth comprising Tetra lauryl orthosilicate as an essential ingredient that enhances strength by forming a covalent bond with a protein in hair.
The present invention also relates to a process for the improved hair care products of the invention.

Background of the invention:
Hair loss is one of the universal problems and it can be temporary or permanent. It can be the result of breakage of hair, hormonal changes, hereditary, medical conditions or aging. 80% of people suffer from hair loss due to the weakening of hair strands.
Mostly, the hair breaks from the weak links formed on the cuticle of the hair strand. If these weak links are connected with each other, the breakage is avoided to a considerable extent.
Dermal Papillae (DP) cells residing at the base of the hair follicle, if decrease below a threshold, the ability of the scalp to produce new hair goes down resulting in hair thinning and hair loss. DP cells are at the base of the hair in the shaft and are responsible for growing the cell numbers and length.
Collagenase is an enzyme activated by UV insult or Reactive Oxygen Species (ROS). An invitro anti-collagenase will protect the collagen fibres which are responsible for holding the DP cells and hair follicles together leading to strong and healthy hair which may prevent breakage or hair fall.
The main component of hair is keratin, which is a hard protein. The common hair components are carbon (50.65%), hydrogen (6.36%), nitrogen (17.4%), sulphur (5%) and oxygen (20.85%). Proteins are composed of peptide bonds that are joined as water is removed between the alpha-carboxyl group of amino acid and the alpha-amino group of the next amino acid. According to the number of peptide-bound amino acids (the number of amino acids in the peptide), those with 2 to 10 are called oligopeptides, those with 10 to 50 are called polypeptides, and those with more than 50 are called proteins. Amino acids, which are the building blocks of proteins, are present in all cells in very small amounts, but are also precursors of proteins.
These hair proteins are a kind of very strong protein under mild conditions such as water or neutral solvents, but when combined with heat generated due to the use of a hair dryer; hair dyeing; different hair treatments including ironing, perming, etc; physical friction in daily life; and hair washing; they may easily be damaged due to these physical/chemical treatments such as sunlight, heat from ironing, adsorption of dirt, exposure to ultraviolet rays, exposure to high and low temperatures, etc. As a result, damaged hair may have problems such as easily fraying, breaking, or tearing as the internal and external proteins are eluted, porosity progresses, and the strength decreases as it becomes rough and may break not only from the scalp i.e. at the root but also at any point on the hair strand.
Thus, hair fall generally occurs due to damage at the root and/or due to breakage at some point on the hair strand.
US 2014161912 publication discloses the composition comprising 10 to 40 % of an Orthosilicate represented by Si(OR)4 wherein R is C1 to C12 alkyl. The composition further comprises oil. This composition is specifically used for treating a condition or disease that requires tissue generation. Specifically, conditions or diseases acne, a puncture wound, and surface lesion due to melanoma or basal cell carcinoma.
According to our knowledge after conducting the prior art search, the problem of breaking or tearing hair strands at any point on the strands other than from the root was not addressed in any of the existing arts. Therefore, there is a need to develop hair care products that will address this aforesaid problem.

Objectives of the present invention:
The main objective of the present invention is to provide improved hair care products to reduce hair fall and increase hair strength and hair growth comprising Tetra lauryl orthosilicate as an essential ingredient that eliminates the problem of breaking or tearing hair strands at any point other than from the scalp or root.
Another objective of the present invention is to provide the improved hair care products that enhance hair strength by forming a covalent bond with proteins available on the hair strands thereby reinforcing the hair.
Another objective of the present invention is to provide the improved hair care products that bridge gaps of the weak links present on the hair strands thereby reinforcing the hair.
Still another objective of the present invention is to provide the improved hair care products that align the cuticles of the hair surface to prevent breakage thereby reinforcing the hair.
Yet another objective of the present invention is to provide the improved hair care products that are non-toxic, non-irritant, odourless, skin safe, and easily miscible with an oil system.
Yet another objective of the present invention is to provide the improved hair care products that are effective at very low concentrations as low as 0.5 to 1 % wt./wt. of Tetra lauryl orthosilicate.
An additional objective of the present invention is to provide a process for the preparation of the improved hair care products to reduce hair fall and increase hair strength and hair growth.

Summary of the invention:
It is surprising to find that the improved hair care products of the present invention effectively bridge gaps of the weak links of the proteins present on hair strands and align the cuticles of hair surface to prevent breakage thereby reinforcing strength of the hair and preventing hair fall or thinning of hair due to breakage as well as increase the hair growth when the products comprise:
at least one active component namely Tetra-lauryl orthosilicate at a very low concentration of 0.5 to 1 % wt./wt. of the composition of the products.
However, when the active component namely Tetra-lauryl orthosilicate is present at a concentration below 0.5 % wt./wt. in the composition of the products, then it is not effectively bridging gaps of the weak links of the proteins present on hair strands nor aligning the cuticles of hair surface thereby not leading to preventing breakage nor reinforcing the hair nor preventing hair fall nor thinning of hair due to breakage.
Further, it is surprisingly found that when the active component namely Tetra-lauryl orthosilicate is present at a concentration above 1 % wt./wt. in the composition of the products, then instead of increasing the efficiency or efficacy of the products, MTT essay method reflected a decrease in preventing breakage by not effectively bridging gaps of the weak links of the proteins present on hair strands nor aligning the cuticles of hair surface nor reinforcing the hair nor preventing hair fall nor thinning of hair.
According to the Collagenase Inhibition Study, Toxicity Profile and Hair Proliferation Assay study, the optimum concentration of active component namely Tetra-lauryl orthosilicate is found to be 0.5 to 1 % wt./wt. of the composition.
It is demonstrated that the products of the invention comprising Tetra lauryl orthosilicate as an essential ingredient forms a covalent bond with a protein in hair thereby bridging the gap of the weak links thereby eliminating the problem of breaking or tearing hair strands at any point other than from the scalp and increasing/reinforcing the strength of the hair and reducing the hair fall. It also increases hair growth as an additional advantage. We also found that the improved hair care products of the invention are non-toxic, non-irritant, odourless, and skin safe.

According to one of the embodiments of the invention, there is provided the improved hair care products to reduce hair fall and increase hair strength and hair growth wherein,
said products comprises:
at least one active component namely Tetra-lauryl orthosilicate.

Typically, the products comprise Tetra-lauryl orthosilicate in the range of 0.5 to 1 % wt./wt. of the composition of the product.
Typically, the improved hair care products are value-added hair oil, hair serum, hair cream, hair wax, etc.
Typically, the improved hair care product, particularly value-added hair oil further comprises oil and suitable additives.
Typically, the oil used in the composition of the invention is selected from castor oil, paraffin oil, coconut oil, aloe vera oil, almond oil, peanut oil, olive oil, sesame oil, shea butter oil, soyabean oil, chamomile oil, geranium oil, jojoba oil, juniper oil, lavender oil, palm oil, sunflower oil, vanilla oil, sweet almond oil, cashew oil, hazelnut oil, macadamia oil, mongongo nut oil, pecan oil, pine nut oil, pistachio oil, walnut oil, avocado oil, cocoa butter oil, corn oil or grapeseed oil.
Typically, the oil used in the value-added hair oil of the invention is coconut oil, Paraffin oil, or a mixture thereof.
Typically, the value-added hair oil comprises coconut oil and Paraffin oil in the proportions of 0 to 100: 100 to 0.
Typically, the value-added hair oil comprises coconut oil and Paraffin oil in the proportions of 50:50.
Typically, the suitable additives used in the value-added hair oil is perfume.

Typically, the hair cream further comprises Tetra-lauryl orthosilicate along with other conventional ingredients.

Typically, the hair wax further comprises Tetra-lauryl orthosilicate along with other conventional ingredients.

Typically, the hair serum further comprises Tetra-lauryl orthosilicate along with other conventional ingredients.

According to another embodiment of the present invention, there is provided a process to prepare the improved hair care products of the invention; wherein the process comprises adding 0.5 to 1 % wt./wt. Tetra-lauryl orthosilicate into the composition of the products and stirring.
Typically, a process to prepare the value-added hair oil comprises adding 0.5 to 1 % wt./wt. Tetra-lauryl orthosilicate and predefined quantity of perfume into a predefined quantity of oil, and mixing the content at 500 rpm for at least 10 to 20 minutes.

According to the application study of the improved hair care products of the invention, it is observed that the gaps of the weak links on the hair strands are bridged and also aligned the cuticles of the hair surface and thereby decreasing hair fall to at least 4 to 25%. Further, the tensile strength study demonstrated that % elongation of break increased to 38.5 %, and break strength (gram force) increased to 116.5 against the control thereby increasing the strength of the hair. Elemental silica deposition study established that hair treated with the hair care products of the invention detected deposition of silica of 0.18 against control having - 0.82. A pilot in-vivo study on hair fall reduction is conducted by using treatment with the improved hair care products of the invention on 8 healthy volunteers for 45 days. Volunteers are asked to apply value-added hair oil of the invention on daily basis and follow their standard regime of hair wash. The fallen hairs are weighed after 15, 28 and 44 days. The results demonstrated at least a reduction in hair fall is 4 %, preferably 4 to 25 %.

Detailed description of the drawings of the invention:
Figure 1 illustrates the SEM analysis image of hair strands with and without treatment using value-added hair oil of the invention.
Figure 2 illustrates the SEM analysis image of hair tresses reflecting of alignment of the cuticles on the surface of the strands with and without treatment using value-added hair oil of the invention.
Figure 3 illustrates a mechanism of action of the value-added hair oil of the invention.
Detailed description of the invention:
The terms “a,” “an,” “the” and similar referents used in the context of describing the invention following claims are to be construed to cover both the singular and the plural, unless otherwise indicated herein or clearly contradicted by context. Recitation of ranges of values herein is merely intended to serve as a shorthand method of referring individually to each separate value falling within the range. Unless otherwise indicated herein, each individual value is incorporated into the specification as if it were individually recited herein. All methods described herein can be performed in any suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (e.g., “such as”) provided herein is intended merely to better illuminate the invention and does not pose a limitation on the scope of the invention otherwise claimed. No language in the specification should be construed as indicating any non-claimed element essential to the practice of the invention.

Certain embodiments of this invention are described herein, including the best mode known to the inventors for carrying out the invention. Of course, variations on these described embodiments will become apparent to those of ordinary skill in the art upon reading the description. The inventor expects skilled artisans to employ such variations as appropriate, and the inventors intend for the invention to be practiced otherwise than specifically described herein. Accordingly, this invention includes all modifications and equivalents of the subject matter recited in the claims appended hereto as permitted by applicable law. Moreover, any combination of the below-described elements in all possible variations thereof is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by context.

Hair loss may occur due to various reasons. To prevent hair loss, primarily Dermal Papillae (DP) cells and Collagenase enzyme are important factors apart from individual’s health issues, use of hair care products, the effect of climatic conditions, etc.

Dermal Papillae (DP) cells residing at the base of the hair follicle, if decrease below a threshold, the ability of the scalp to produce new hair goes down resulting in hair thinning, and hair loss. DP cells are at the base of the hair in the shaft and are responsible for growing the cell numbers and length.
Collagenase is an enzyme activated by UV insult or ROS. An invitro anti-collagenase will protect the collagen fibers which are responsible for holding the DP cells and hair follicles together leading to strong and healthy hair which may prevent breakage or hair fall.

Before analysing the active component namely Tetra-lauryl orthosilicate for treatment of hair loss due to gaps or breakage created due to the weak links available on the hair strands or due to the presence of unaligned cuticles on the hair surface, it is important to test toxicity of the material, hence the in-vitro toxicity is analysed on Human Dermal Fibroblasts (HDF) cells.

“Cell Proliferation Assay of the sample on Human Papilla Cell Line” is performed in full compliance with the NCI Guidelines for evaluation of cytotoxicity and the SRC protocol number SRC/BT/DPC/01 i.e. MTT assay (References: Madaan, A., Verma, R., Singh, A.T. and Jaggi, M., 2018. Review of hair follicle dermal papilla cells as in vitro screening model for hair growth. International Journal of cosmetic science, 40(5), pp.429-450.) It is designed to study the Cytotoxicity potential of the investigational sample in terms of the IC50 values, derived from the dose response curve.

MTT assay is performed in a 96-well tissue culture plate. The duration of the assay is 4 days. The cells are seeded into the plate and after they sub-confluent they are treated with the test material for 24 hrs. The MTT assay is a metabolic assay. Cellular damage inevitably results in loss of the ability of the cell to maintain and provide energy for metabolic cell function and growth. Yellow MTT (3-(4, 5-Dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide, a tetrazole) reduces to purple formazan in the mitochondria of living cells. The absorbance of this colored solution is quantified by measuring at 570 nm by a spectrophotometer. This reduction takes place only when mitochondrial reductase enzymes are active, and therefore conversion can be directly related to the number of viable (living) cells. Mitochondrial dehydrogenases of viable cells cleave the tetrazolium ring, yielding purple MTT formazan crystals which are insoluble in aqueous solutions. An increase in cell number results in an increase in the amount of MTT formazan formed and an increase in absorbance. It is thus possible to distinguish between viable, damaged or dead cell, which is the basis of this assay. The intensity of the colour is directly proportional to the amount of the live cells, which is an indication of cell viability.

100 mg/ml of test samples are prepared in 1% DMSO. After solubilizing, different concentrations of 0.05%, 0.025%, 0.0125%, 0.00625% and 0.003125% of Tetra-lauryl orthosilicate in 1% DMSO are prepared. All test samples of Tetra-lauryl orthosilicate are freshly prepared just before use. The experiment is repeated thrice.
According to the results, it is observed that DPC Cell proliferation capacity is decreased with an increase in the concentration of the active component namely Tetra-lauryl orthosilicate in the test solution.
According to the results in respect of DPC Cell proliferation capacity;
the concentration 0.003125 % of Tetra-lauryl orthosilicate demonstrated cell viability of 132.60 %, which exhibited 32.60 % more proliferation as compared to cell control;
the concentration 0.00625 % of Tetra-lauryl orthosilicate demonstrated cell viability of 119.13 %, which exhibited 19.30 % more proliferation as compared to cell control;
the concentration 0.0125 % of Tetra-lauryl orthosilicate demonstrated cell viability of 114.78 %, which exhibited 14.78 % more proliferation as compared to cell control;
the concentration 0.025 % of Tetra-lauryl orthosilicate demonstrated cell viability of 101.739 %, which exhibited 1.739 % more proliferation as compared to cell control; and
the concentration 0.05 % of Tetra-lauryl orthosilicate demonstrated cell viability of 96.522 %, which exhibited 3.478 % less proliferation as compared to cell control.

Collagenase Inhibition capacity is performed in full compliance with the NCI Guidelines for evaluation of cytotoxicity and the SRC protocol no. SRC/BT/5401-10-15.
Test samples of 0.05 %, 0.075 %, 0.10 %, 0.25 % and 0.50 % of Tetra-lauryl orthosilicate in Tricine buffer are prepared. All test samples of Tetra-lauryl orthosilicate are freshly prepared just before use. The experiment is repeated thrice.
According to the results in respect of Collagenase Inhibition capacity;
the concentration 0.05 % of Tetra-lauryl orthosilicate demonstrated Collagenase Inhibition of 1.302%.
the concentration 0.075 % of Tetra-lauryl orthosilicate demonstrated Collagenase Inhibition of 33.724%,
the concentration 0.10 % of Tetra-lauryl orthosilicate demonstrated Collagenase Inhibition of 65.2344%,
the concentration 0.25 % of Tetra-lauryl orthosilicate demonstrated Collagenase Inhibition of 88.2812%,
the concentration 0.50 % of Tetra-lauryl orthosilicate demonstrated Collagenase Inhibition of 92.5781%
Thus, it is observed that there is a linear increase in Collagenase inhibition with increase in the concentration of the active component namely Tetra-lauryl orthosilicate in the test solution.

Toxicity Profile is performed in full compliance with the NCI Guidelines for evaluation of cytotoxicity and the SRC protocol no. SRC/BT/HDF/01*
Test samples of 0.0125 %, 0.025 %, 0.05 %, and 0.100 % of Tetra-lauryl orthosilicate in 1% DMSO are prepared. All test samples of Tetra-lauryl orthosilicate are freshly prepared just before use. The experiment is repeated thrice.
According to the results in respect of Toxicity Profile;
the concentration 0.0125 % of Tetra-lauryl orthosilicate demonstrated 98.485% cell viability;
the concentration 0.025 % of Tetra-lauryl orthosilicate demonstrated 106.081% cell viability
the concentration 0.05 % of Tetra-lauryl orthosilicate demonstrated 92.828% cell viability %; and
the concentration 0.10 % of Tetra-lauryl orthosilicate demonstrated 73.737% cell viability
Thus, it is observed that the active component namely Tetra-lauryl orthosilicate demonstrated safe profile when tested on Human Dermal Fibroblasts in vitro.

According to the results obtained in the DPC Cell proliferation capacity, Collagenase Inhibition capacity and Toxicity Profile, we observed that the optimum concentration of the active component namely Tetra-lauryl orthosilicate in the hair care products of the invention is 0.5 to 1 % wt./wt.

Accordingly, one of the embodiments of the present invention, there is provided improved hair care products to reduce hair fall, and increase hair strength and hair growth;
said products comprising at least one active component namely Tetra-lauryl orthosilicate.
Preferably, the products of the invention comprise 0.5 to 1 % wt./wt. at least one active component namely Tetra-lauryl orthosilicate.

According to the inventions, the improved hair care products are value-added hair oil, hair serum, hair wax, hair cream, etc.

Another embodiment of the present invention, there is provided a value-added hair oil as the improved hair care product wherein said product further comprises oil and suitable additives.
The oil used in the value-added hair oil of the invention is selected from castor oil, paraffin oil, coconut oil, aloe vera oil, almond oil, peanut oil, olive oil, sesame oil, shea butter oil, soyabean oil, chamomile oil, geranium oil, jojoba oil, juniper oil, lavender oil, palm oil, sunflower oil, vanilla oil, sweet almond oil, cashew oil, hazelnut oil, macadamia oil, mongongo nut oil, pecan oil, pine nut oil, pistachio oil, walnut oil, avocado oil, cocoa butter oil, corn oil or grapeseed oil
Preferably, the oil used in the product of the invention is Coconut oil, Paraffin oil or a mixture thereof.
The coconut oil and paraffin oil used in the value-added hair oil is in the proportion of 0 to 100: 100 to 0.
Preferably, the coconut oil and paraffin oil used in the value-added hair oil is in the proportion of 50: 50.
Preferably, the suitable additive used in the value-added hair oil is perfume.

Yet another embodiment of the invention, there is provided a process to prepare the improved hair care products of the invention.
In this process, a predefined amount of at least one active component namely Tetra-lauryl orthosilicate is added in predefined amount of conventional ingredients and suitable additives and the mixture is stirred for at least 10-20 minutes at the ambient temperature of 30-35°C.
Preferably, at least 0.5 wt./wt. of Tetra-lauryl orthosilicate is added.
More preferably, 0.5 to 1 wt./wt. of Tetra-lauryl orthosilicate is added.

The improved hair care products namely, value-added hair oil, hair cream, hair wax, hair serum, etc are prepared.

In one of the embodiments of the present invention, one of the improved hair care products of the invention namely value-added oil comprising at least one active component namely Tetra-lauryl orthosilicate is tested on the hair for its performance.
Typically, the value-added hair oil comprises 0.5 to 1 % wt./wt. Tetra-lauryl orthosilicate, Oil and suitable additive including Perfume.
Typically, the value-added hair oil comprises 0.5 to 1 % wt./wt. of Tetra-lauryl orthosilicate, 98.7 to 99.2 % wt./wt. of Oil and 0.3 % wt./wt. suitable additive including Perfume.

The oil used in the value-added hair oil of the invention is selected from castor oil, paraffin oil, coconut oil, aloe vera oil, almond oil, peanut oil, olive oil, sesame oil, shea butter oil, soyabean oil, chamomile oil, geranium oil, jojoba oil, juniper oil, lavender oil, palm oil, sunflower oil, vanilla oil, sweet almond oil, cashew oil, hazelnut oil, macadamia oil, mongongo nut oil, pecan oil, pine nut oil, pistachio oil, walnut oil, avocado oil, cocoa butter oil, corn oil or grapeseed oil
Preferably, the oil used in the product of the invention is Coconut oil, Paraffin oil or a mixture thereof.
The Coconut oil and Paraffin oil used in the value-added hair oil is in the proportion of 0 to 100: 100 to 0.
Preferably, the Coconut oil and Paraffin oil used in the value-added hair oil is in the proportion of 50: 50.

One of the examples of value-added hair oil comprises Coconut oil, Tetra-lauryl orthosilicate and Perfume.

The value-added hair oil is prepared by adding a predefined quantity of at least one active component namely Tetra-lauryl orthosilicate and Perfume into a predefined quantity of Oil, and mixing the content at 500 rpm for at least 10 to 20 minutes.

In yet another embodiment of the present invention, another improved hair care product of the invention namely hair serum comprising at least one active component namely Tetra-lauryl orthosilicate is tested on the hair for its performance.
Typically, the hair serum comprises Tetra-lauryl orthosilicate along with other conventional ingredients.
One of the examples of the hair serums comprises:
Phase A consisting Trehalose, Hydroxyethyl cellulose, Ethylenediamine tetra acetic acid, Polyglycerin and DM water;
Phase B consisting Cetostearyl alcohol, Glycerol monostearate, and Mineral oil;
Phase C consisting Polydimethyl siloxane, Isododecane & Dimethicone and Tetra-lauryl orthosilicate; and
Phase D consisting Sodium benzoate and Perfume.
This hair serum is prepared by (1) mixing Phase A ingredients in a predefined amount at 500 rpm followed by heating the Phase A mixture to 70°C; (2) heating Phase B ingredients in a predefined amount at 70°C followed by slow mixing; (3) adding Phase B content to Phase A content under mixing at 1000 rpm followed by mixing the whole content at 4000 rpm with high shear mixer; (4) adding Phase C ingredients in a predefined amount to the reaction mixture obtained in step (3) under moderate shear (500 rpm); (5) cooling down the mixture of step (4) to 40°C; (6) adding Phase D ingredients in a predefined amount one at a time to the mixture obtained at step (5) under moderate shear (500 rpm) to obtain hair serum; and (7) optionally, adjusting pH of the serum to 5 to 5.5.

Another example of the hair serums comprises:
Phase A consisting Isododecane, Dimethicone, Tetra-lauryl orthosilicate and Vinyl dimethicone; and
Phase B consisting Phenyl trimethicone, Cyclopentasiloxane, and Perfume.
The hair serum is prepared by (1) mixing Phase A ingredients in a predefined amount at 300 rpm for at least of 10 to 20 minutes; (2) mixing Phase B ingredients in a predefined amount at 300 rpm for at least of 10 to 20 minutes; and (3) adding the Phase B to the Phase A under moderate shear of 300 rpm.

In still another embodiment of the present invention, yet another improved hair care product of the invention namely hair cream comprising at least one active component namely Tetra-lauryl orthosilicate is tested on the hair for its performance.
Typically, the hair cream comprises Tetra-lauryl orthosilicate along with other conventional ingredients.
One of the examples of the hair creams comprises:
Phase A consisting Polysorbate 20, Propylene glycol, Ethylenediamine tetra acetic acid, Triethanol amine and Hydroxyethyl cellulose;
Phase B consisting DM Water, Cetostearyl alcohol, Cetyl alcohol, Glycerol monostearate, Beewax and Mineral oil;
Phase C consisting of Polysilsesquioxane, Disunfloweroylethyl, Sodium propyl paraben and Tetra-lauryl orthosilicate; and
Phase D consisting of Sodium benzoate and Perfume.
This hair cream is prepared by (1) mixing Phase A ingredients in a predefined amount at 500 rpm with simultaneous heating of mixture to 70°C; (2) heating Phase B ingredients in a predefined amount at 70°C followed by slow mixing; (3) adding Phase B content to Phase A content under mixing at 1000 rpm followed by mixing the whole content at 4000 rpm with high shear mixer; (4) adding Phase C ingredients in a predefined amount to the reaction mixture obtained in step (3) under moderate shear (500 rpm); (5) cooling down the mixture of step (4) to 40°C; (6) adding Phase D ingredients in a predefined amount one at a time to the mixture obtained in step (5) under moderate shear (500 rpm) to obtain hair cream; and (7) optionally, adjusting pH of the serum to 5.5 to 6.

In still another embodiment of the present invention, another improved hair care product of the invention namely hair wax comprising at least one active component namely Tetra-lauryl orthosilicate is tested on the hair for its performance.
Typically, the hair wax comprises Tetra-lauryl orthosilicate along with other conventional ingredients.
One of the examples of the hair wax comprises:
Phase A consisting 2-Amino-2-methylpropan, Polyglycerin, and DM Water;
Phase B consisting Ceteth-20, Cetreath-30, Cetreth 20, Argan oil, and Ethylhexylglycerin; and
Phase C consists of Tetra-lauryl orthosilicate, Polyquaternium-6, Tetradecanoic acid isopropyl and Disunfloweroylethyl Dimonium.
The hair wax is prepared by (1) mixing Phase A ingredients in a predefined amount at 500 rpm with simultaneous heating of mixture to 70°C; (2) heating Phase B ingredients in a predefined amount at 70°C followed by slow mixing; (3) adding Phase B content to Phase A content under mixing at 1000 rpm followed by mixing the whole content at 4000 rpm with high shear mixer; (4) adding Phase C ingredients in a predefined amount to the reaction mixture obtained in step (3) under moderate shear (500 rpm); (5) cooling down the mixture of step (4) to 30°C; (6) adding Phase D ingredients in a predefined amount one at a time to the mixture obtained in step (5) under moderate shear (500 rpm) to obtain hair wax; and (7) adjusting pH of the serum to 6.0 to 6.5.

The hair care products namely, value-added hair oil, hair serum, hair cream and hair wax; comprising Tetra-lauryl orthosilicate are tested for hair tensile strength study, elemental silica deposition study, efficacy in-Vivo hair fall reduction study on human hair tresses, and SEM analysis. Water and coconut oil are used as a control for these studies.

Tensile Strength Study:
The hair care products comprising 1 % wt./wt. of Tetra-lauryl orthosilicate, Water (control 1), and Coconut oil (control 2) are applied to hair tresses every day in the evening for 7 days. During the test, the treated hair tresses samples are washed with 15 % Sodium lauryl ether sulphate (SLES) every day morning and allowed to air dry throughout the day. These treated hair tresses samples are subjected to elongation and breakage study using Universal Tensile tester after 7 days.
According to the results obtained, the hair tresses samples are treated with hair care products comprising 1 % wt./wt. of Tetra-lauryl orthosilicate demonstrated (%) elongation of break of 38.5 % and break strength of 116.5 gram/force while that of the hair tresses samples treated with control 1 and control 2 demonstrated (%) elongation of break of 35.7 and 35 respectively and break strength of 96.8 and 93.9 respectively.

Elemental Silica deposition Study:
The elemental silica deposition study is carried out by washing hair tresses samples to strip-off residual Silica, if any. The hair care products comprising 1 % wt./wt. of Tetra-lauryl orthosilicate, Water (control 1), and Coconut oil (control 2) are applied to hair tresses samples for 12 days. With minimum exposure of 12 hours to the treatment, the treated tresses samples are washed every day with 15 % SLES. The residual Silica is analysed by XRF. According to the results, it is observed that the hair tresses samples treated with hair care products comprising 1 % wt./wt. of Tetra-lauryl orthosilicate have shown positive deposition of Silica on the hair strands as compared to Water (control 1), and Coconut oil (control 2). The silica deposition promotes the strengthening of the hair strands.

In-Vivo Hair Fall Reduction (Hair loss) Study:
This study is conducted on eight healthy volunteers of age between 19 to 46 for 45 days. Volunteers are asked to apply hair care products comprising 1 % wt./wt. of Tetra-lauryl orthosilicate daily and follow their standard regime of hair wash. The fallen hair is measured in terms of weighed of hair loss on days 0, 15, 28 and 44 days of treatment. According to the results, the reduction in hair loss/fall is observed which is in the range of 4 to 25 % in 45 days.

Scanning Electron Microscope (SEM) Analysis:
The hair tresses samples are analysed by scanning Electron Microscope analysis upon treatment with hair care products comprising Tetra-lauryl orthosilicate and with Oil (i.e. control without Tetra-lauryl orthosilicate). The image of the hair strand as illustrated in Figure 1 displays raised cuticle and breakage that exists on the surface of the hair strand. It also reflects weak links present in form of unaligned cuticles, raised cuticles or breakages on the hair strand surface with and without treatment.
Figure 2 illustrates hair cuticles are aligned on treatment with value-added oil comprising the Tetra-lauryl orthosilicate while hair cuticles are not aligned on treatment with control (i.e. without tetra-lauryl orthosilicate).
Figure 3 illustrates the mechanism of action of hair strengthening on treatment with value-added oil comprising the Tetra-lauryl orthosilicate where functional groups of orthosilicate react with proteins available on the weak links or breakages existing over the surface of the hair strands and forming covalent bonds thereby causing cementing and thus strengthening hair.

Thus, it is demonstrated that the gaps of the weak links or breakages present on the hair strands are bridged simultaneously and it also aligned cuticles of the hair surface thereby decreasing hair fall to at least 4 to 25 %. Further, the hair strength study exhibited that % elongation of break increased to 38.5 %, and break strength increased to 116.5 gram force against the control thereby increasing the strength of hair. Elemental silica deposition study of residual silica post washing demonstrated that hair treated with the improved hair care products of the invention detected Silica of 0.18 against control having - 0.82.

The present invention can be illustrated with the below mentioned examples and comparative examples but not by way of limitations. In other words, exemplary illustrations of the operation of the present invention, the practice of its formulation and rendering of the disclosed process are described in the following examples. In addition to the preferred modes of operation, a practitioner of sufficient skill in the art will appreciate that the meets and bounds of the present invention are not limited by the specific instances described herein, rather are defined by the equivalents provided by the claims of the present invention.

Examples:
The following improved hair care products of the invention namely value-added hair oil, hair cream, hair wax, and hair serum were prepared according to the formulations in Table 1:

Table 1: Formulations of value-added hair oil, hair cream, hair wax, hair serum
Hair care products Ingredients % wt./wt. Properties of hair care products
Value added Hair oil (I) Coconut oil
Tetra-lauryl orthosilicate
Perfume 98.7
1
0.3 Viscosity: 78 cps
State: liquid.
Value added Hair oil (II) Paraffin oil
Tetra-lauryl orthosilicate
Perfume 98.7
1
0.3 Viscosity: 53 cps
State: liquid.
Value added Hair oil (III) Coconut oil and Paraffin oil (50:50)
Tetra-lauryl orthosilicate
Perfume 98.7
1
0.3 Viscosity: 63 cps
State: liquid.
Value added Hair oil (IV) Coconut oil
Tetra-lauryl orthosilicate
Perfume 99.2
0.5
0.3 Viscosity: 78 cps
State: liquid.
Value added Hair oil (V) Paraffin oil
Tetra-lauryl orthosilicate
Perfume 99.2
0.5
0.3 Viscosity: 53 cps
State: liquid.
Value added Hair oil (VI) Coconut oil and Paraffin oil (50:50)
Tetra-lauryl orthosilicate
Perfume 99.2
0.5
0.3 Viscosity: 62 cps
State: liquid.
Hair Serum I Phase A
Trehalose,
Hydroxyethyl cellulose
Ethylenediamine tetra acetic acid
Polyglycerin
DM water.
Phase B
Cetostearyl alcohol
Glycerol monostearate
Mineral oil.
Phase C
Polydimethyl siloxane
Isododecane & Dimethicone
Tetra-lauryl orthosilicate
Phase D
Sodium benzoate
Perfume.
2
0.5
0.12
5
q.s. to 100

3
0.5
1.5

1.5
1
1

0.5
0.5 pH- 5.5
Viscosity-974.0 cps
State: Milky White liquid
Hair Serum II Phase A
Isododecane
Dimethicone
Tetra-lauryl orthosilicate
Vinyl dimethicone
Phase B
Phenyl trimethicone
Cyclopentasiloxane
Perfume.
43.60
48
1
1

1
5
0.40 pH- 5.5 to 6
Viscosity-170.3 cps
State: Transparent liquid
Hair Cream Phase A
Polysorbate 20
Propylene glycol
Ethylenediamine tetra acetic Acid
Triethanol amine
Hydroxyethyl cellulose.
Phase B
DM Water
Cetostearyl alcohol
Cetyl alcohol
Glycerol monostearate
Beewax
Mineral oil.
Phase C
Polysilsesquioxane
Disunfloweroylethyl
Sodium propyl paraben
Tetra-lauryl orthosilicate
Phase D
Sodium benzoate
Perfume.
2.00
5.00
0.12
0.50
0.50

q. s. to 100
3.00
0.50
0.50
2.00
5.00

0.15
1.00
0.50
1.00

0.50
0.50 pH- 5.5 to 6
Viscosity-18400 cps
State: White paste
Hair Wax Phase A
2-Amino-2-methylpropan
Polyglycerin
DM Water
Phase B
Ceteth-20
Cetreath -30
Cetreth 20
Argan oil
Ethylhexylglycerin
Phase C
Tetra-lauryl orthosilicate
Polyquaternium-6
Tetradecanoic acid isopropyl
Disunfloweroylethyl dimonium
1.10
5.00
q. s. to 100

4.00
15.00
5.00
0.20
0.70

1.00
10.00
4.00
2.00 pH- 5.5
Viscosity-9-100 cps
State: Solid cream

Value-added hair oils I to VI were prepared by adding the Tetra-lauryl orthosilicate and perfume into oil in the quantities specified in Table 1. The content was mixed at 500 rpm for at least 10 to 20 minutes.

Hair serum I was prepared by (1) mixing Phase A ingredients in the amount specified in Table 1 at 500 rpm followed by heating the Phase A mixture to 70°C; (2) heating Phase B ingredients in the amount specified mixture in Table 1 at 70°C followed by slow mixing; (3) adding Phase B content to Phase A content under mixing at 1000 rpm followed by mixing the whole content at 4000 rpm with high shear mixer (Silverson); (4) adding Phase C ingredients in the amount specified in Table 1 to the reaction mixture obtained in step (3) under moderate shear (500 rpm); (5) cooling down the mixture obtained in step (4) to 40°C; (6) adding Phase D ingredients in the amount specified in Table 1 one at a time to the obtained in step (5) under moderate shear (500 rpm) to obtain hair serum; and (7) optionally, adjusting pH of the serum to 5 to 5.5.

Hair serum II was prepared by (1) mixing Phase A ingredients in the amount specified in Table 1 at 300 rpm for at least 10 to 20 minutes; (2) mixing Phase B ingredients in the amount specified in Table 1 at 300 rpm for at least 10 to 20 minutes; and (3) adding the Phase B content to Phase A content under moderate shear of 300 rpm to obtain hair serum; and (4) optionally, adjusting pH of the serum to 5.5 to 6.

Hair cream was prepared by (1) mixing Phase A ingredients in the amount specified in Table 1 at 500 rpm with simultaneous heating of mixture to 70°C; (2) heating Phase B ingredients in the amount specified in Table 1 at 70°C followed by slow mixing; (3) adding Phase B content to Phase A content under mixing at 1000 rpm followed by mixing the whole content at 4000 rpm with high shear mixer (Silverson); (4) adding Phase C ingredients in the amount specified in Table 1 to the reaction mixture obtained in step (3) under moderate shear (500 rpm); (5) cooling down the mixture to 40°C; (6) adding Phase D ingredients in the amount specified in Table 1 one at a time to the mixture obtained in step (5) under moderate shear (500 rpm) to obtain hair cream; and (7) optionally, adjusting pH of the cream to 5.5 to 6.

Hair wax was is prepared by (1) mixing Phase A ingredients in the amount specified in Table 1 at 500 rpm with simultaneous heating of mixture to 70°C; (2) heating Phase B ingredients in the amount specified in Table 1 at 70°C followed by slow mixing; (3) adding Phase B content to Phase A content under mixing at 1000 rpm followed by mixing the whole content at 4000 rpm with high shear mixer (Silverson); (4) adding Phase C ingredients in the amount specified in Table 1 to the reaction mixture obtained in step (3) under moderate shear (500 rpm); (5) cooling down the mixture to 30°C; (6) adding Phase D ingredients in the amount specified in Table 1 one at a time to the mixture obtained in step (5) under moderate shear (500 rpm) to obtain hair wax; and (7) adjusting pH of the serum to 6.0 to 6.5.

Value-added hair oil I was tested for hair tensile strength study, elemental silica deposition study and efficacy in-Vivo hair fall reduction study on human hair tresses samples by using Water and Coconut oil as a control.

Hair tensile strength study on human hair tresses samples:
Value-added hair oil I, Water (Control 1) and Coconut oil (Control 2) were applied to hair tresses samples every day in the evening. The oil samples were allowed to reside on the tresses samples overnight. Every day the hair tresses samples were washed with 15 % Sodium lauryl ether sulphate and allowed to air dry throughout the day. This treatment was continued for 7 days. The hair tresses samples were then subjected to tensile strength particularly % elongation and % breakage study using a Universal Tensile tester. The results are given in Table 2.

Table 2: Results of tensile strength study
Sr. No. Treatment Elongation at break % Breaking strength Gram Force
1 Water (Control 1) 35.7 96.8
2 Coconut oil (Control 2) 35 93.9
3 Value-added hair oil I 38.5 116.5

According to the study, the hair tresses samples treated with Value-added hair oil I demonstrated excellent enhancement of elongations at break and breaking strength as compared to that of samples treated with Water (Control 1) and Coconut oil (Control 2). Thus, the hair strength of the sample increased upon treatment with the Value-added hair oil of the invention.

Elemental Silica deposition Study:
Value-added hair oil I, Water (Control 1), and Coconut oil (Control 2) were used to perform this study. The elemental silica deposition study was carried out by washing hair tresses samples to strip-off residual Silica, if any. Value-added hair oil I, Water, and Coconut oil were applied to hair tresses samples for 12 days. With minimum exposure of 12 hours to the treatment, the treated tresses samples were washed every day with 15 % Sodium lauryl ether sulphate. The residual Silica was analysed by XRF and the results of the same are illustrated in Table 3.

Table 3: Results of Elemental Silica deposition by XRF

Sr. No. Treatment Silica deposition
1 Value-added hair oil II 0.16
2 Water (Control 1) - 0.14
3 Coconut oil (Control 2) - 0.82

According to the results illustrated in Table 4, the hair tresses samples found silica deposition when they were treated with Value-added hair oil I while the hair tresses samples found a reduction in silica concentration when they were treated with Water and Coconut oil. The silica deposition promotes the strengthening of the hair strands.

In-Vivo Hair Fall Reduction (Hair loss) Study
This study was conducted on eight healthy volunteers of age between 19 to 46 for 45 days by using Value-added hair oil I. Volunteers were asked to apply hair oil on daily basis and follow their standard regime of hair wash. The fallen hair was collected during sleeping, washing hair or combing hair and this was measured in terms of weight of hair loss on days 0, 15, 28, and 44 days of treatment. The results of this study are illustrated in Table 4.

Table 4: Results of In-Vivo Hair Fall Reduction (Hair loss)
Volunteer No. and Age Day 0 Day 15 Day 28 Day 36 Day 45 % reduction in hair fall/loss
No. 1
Age 40 3.20 2.61 2.51 2.42 2.40 25
No. 2
Age 36 2.61 2.45 2.34 2.35 2.30 11.88
No. 3
Age 19 2.71 2.61 2.45 2.42 2.45 9.59
No. 4
Age 35 2.64 2.59 2.39 2.37 2.35 9.96
No. 5
Age 38 2.73 2.60 2.50 2.51 2.52 7.69
No. 6
Age 27 2.46 2.40 2.39 2.37 2.35 4.47
No. 7
Age 32 2.45 2.42 2.39 2.39 2.35 4.08
No. 8
Age 46 2.49 2.48 2.35 2.35 2.33 6.43

According to the results of Table 4, the reduction in hair loss/fall was found to be in the range of 4 to 25 % in 45 days.

Scanning Electron Microscope (SEM) Analysis:
The hair tresses samples were analysed by the SEM analysis with and without treatment with Value-added oil I. The image of the hair strand as illustrated in Figure 1 displays raised cuticle and breakage that exists on the surface of the hair strand without treatment. It also reflects weak links present in form of unaligned cuticles, raised cuticles or breakages on the hair strand surface without treatment. It also reflects no weak links, no raised cuticles or breakage and aligned cuticles on the hair strand surface with treatment using value-added hair oil (I) of the invention.
Figure 2 illustrates hair cuticles are aligned with treatment with Value-added oil I while hair cuticles are not aligned without treatment.
Figure 3 illustrates the mechanism of action of hair strengthening by using the Value-added hair oil I where functional groups of orthosilicate reacted with proteins available on the weak links or breakages that exist over the surface of the hair strands and formed covalent bonds thereby causing cementing and thus strengthening hairs.

Thus, Value-added hair oil I decreased hair fall and increased hair strength as well as increased hair growth.
Similarly, other hair care products, namely Value-added hair oils II to VI; Hair serum I and II, Hair cream and Hair wax comprising Tetra lauryl orthosilicate were tested for the hair strength and hair loss and hair growth. The results were found to be similar to the Value-added hair oil II.

Thus, the improved hair care products of the invention decreased hair fall and increased hair strength as well as increased hair growth.
, Claims:We claim:

1. Improved hair care products to reduce hair fall and to increase hair strength and hair growth;
said products comprising at least one active component namely Tetra-lauryl orthosilicate.
2. The products as claimed in claim 1, wherein the products comprise 0.5 to 1 % wt./wt. Tetra-lauryl orthosilicate.
3. The products as claimed in claim 1, wherein the products are value-added hair oil, hair cream, hair wax and hair serum.
4. A value-added hair oil as claimed in claim 3, wherein the value-added hair oil comprises at least one active component namely Tetra-lauryl orthosilicate, Oil, and suitable additives including Perfume.
5. The value-added hair oil as claimed in claim 4, wherein the Oil is selected from castor oil, paraffin oil, coconut oil, aloe vera oil, almond oil, peanut oil, olive oil, sesame oil, shea butter oil, soyabean oil, chamomile oil, geranium oil, jojoba oil, juniper oil, lavender oil, palm oil, sunflower oil, vanilla oil, sweet almond oil, cashew oil, hazelnut oil, macadamia oil, mongongo nut oil, pecan oil, pine nut oil, pistachio oil, walnut oil, avocado oil, cocoa butter oil, corn oil or grapeseed oil.
6. The value-added hair oil as claimed in claim 5, wherein the oil used in the composition is coconut oil, Paraffin Oil and a mixture thereof.
7. A hair cream as claimed in claim 3, wherein the hair cream comprises Tetra-lauryl orthosilicate along with other conventional ingredients.
8. A hair wax as claimed in claim 3, wherein the hair wax comprises Tetra-lauryl orthosilicate along with other conventional ingredients.
9. A hair serum as claimed in claim 3, wherein the hair serum comprises Tetra-lauryl orthosilicate along with other conventional ingredients.
10. A process to prepare the hair care products as claimed in any of the preceding claims; wherein the process comprises adding 0.5 to 1 % wt./wt. Tetra-lauryl orthosilicate to the ingredients of the products followed by stirring.
11. A process to prepare the value-added hair oil as claimed in claims 4 to 6 wherein the process comprises adding 0.5 to 1 % wt./wt. Tetra-lauryl orthosilicate and predefined quantity of Perfume into a predefined quantity of Oil, and mixing the content at 500 rpm for at least 10 to 20 minutes.