Sign In to Follow Application
View All Documents & Correspondence

“Composition For Taste Masking Related To Allicin And Process Thereof”

Abstract: The present invention belongs to the field of nutraceuticals and is specifically related to the taste masking of Allicin and the process thereof. In particular the present disclosure provides an allicin taste masking composition and preparation method thereof. Further invention relates to allicin taste masking nutraceutical composition comprising various complexes such as ion exchange resin, beta cyclodextrins, and synergistic forms of Guar gum and Shilajit (Fulvic acid). Another invention belongs to ion exchange resin and beta cyclodextrins methods use chemical constituents, while synergistic forms of Guar gum and shilajit are natural phytoconstituents. All three methods are evaluated and we concluded that the processing time, bioavailability and taste masking effects are better using the natural phyto constituent than using a chemical mixture. Allicin: Guar gum: Shilajit (Fulvic acid) complexes are evaluated for their structural characteristics by XRPD and DSC. The evaluation of taste masking and odor masking are done using in vitro such as the dissolution method and in vivo techniques such as the determination of bitterness threshold concentration. Micromalatic properties of Guar gum: Shilajit complex with Allicin is also evaluated and found satisfactory. The mixture ratio amount of additives in Allicin: Guar gum: Shilajit is lower than chemical complexes.

Get Free WhatsApp Updates!
Notices, Deadlines & Correspondence

Patent Information

Application #
Filing Date
07 April 2023
Publication Number
41/2024
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application

Applicants

Gplife healthcare Pvt Ltd
GPLIFE HEALTHCARE PVT LTD 705-706, Orbit-1, building near RRTM Market, Punagam Saroli Road, Surat-395010 Email : account@gplife.in

Inventors

1. Dr. Shridhar Pandya
GPLIFE HEALTHCARE PVT LTD 705-706, Orbit-1, building near RRTM Market, Punagam Saroli Road, Surat-395010 Email : account@gplife.in
2. Mr. Chetan Savaliya
GPLIFE HEALTHCARE PVT LTD 705-706, Orbit-1, building near RRTM Market, Punagam Saroli Road, Surat-395010 Email : account@gplife.in

Specification

DESC:FIELD OF THE INVENTION
The present invention belongs to the field of nutraceuticals and is specifically related to the taste masking of Allicin and the process thereof. In particular the present disclosure provides an allicin taste masking composition and preparation method thereof. Further invention relates to allicin taste masking nutraceutical composition comprising various complexes such as ion exchange resin, beta cyclodextrins, and synergistic forms of Guar gum and Shilajit (Fulvic acid). Another invention belongs to ion exchange resin and beta cyclodextrins methods use chemical constituents, while synergistic forms of Guar gum and shilajit are natural phytoconstituents.
BACKGROUND OF INVENTION
Allicin is an active organosulfur compound extracted from the bulbs of garlic, a plant of the genus Liliaceae. Allicin is also known as Diallyl thiosulfinates having three thio-allyl ether class compounds. Allicin has many pharmacological effects such as anti-inflammatory, antibacterial, antiviral, anti-cancer, blood pressure lowering, blood lipid-lowering, anticoagulant, prevents arteriosclerosis, prevents and treats cardiovascular and cerebrovascular diseases, and has extremely high health care value. Allicin has the effect of elevating gastric secretion and gastrointestinal motility, stimulating appetite and promoting digestion. The disadvantage of allicin is its chemical properties as it is volatile, unstable, and decomposes when it encounters heat and alkali, as well as it has strong stimulation to the human mucous membrane.

Allicin injection is unstable in nature and has many side effects such as irritation to blood vessels, local vasculitis and pain during injection, which limits the application of the drug. Allicin has a peculiar odor and taste which affects drug compliance. In order to mask the bad taste of allicin, flavors, sweeteners, and fragrances, are incorporated in formulations, but many times it fails to mask the bad smell of allicin. At present, there are many chemical methods to mask the smell and taste of allicin but some of them are very complicated, cost-effective and lower the activity of allicin. Therefore it is required to develop a process to effectively mask its irritating smell and taste without compromising the activity of allicin.
Nutraceuticals refer to products derived from food sources with extra health benefits in addition to the basic nutritional value found in foods. Allicin is a compound found in garlic that is associated with various health benefits, including antimicrobial and antioxidant properties. However, allicin has a pungent odor and a strong, spicy taste, which can be unpleasant for some individuals.

Taste masking is a process used to cover up or neutralize the unpleasant taste of certain compounds in order to improve palatability and increase patient compliance. In the case of allicin, taste masking techniques may be employed to make nutraceutical formulations containing garlic more palatable.

US9931305B2 discloses rapid dissolve thin film drug delivery compositions for the oral administration of active components. The active components are provided as taste-masked or controlled-release coated particles uniformly distributed throughout the film composition. The compositions may be formed by wet casting methods, where the film is cast and controllably dried, or alternatively by an extrusion method.

US20190380973A1 discloses rapid dissolve thin film drug delivery compositions for the oral administration of active components. The active components are provided as taste-masked or controlled-release coated particles uniformly distributed throughout the film composition. The compositions may be formed by wet casting methods, where the film is cast and controllably dried, or alternatively by an extrusion method.

Journal of food science (J. Food Sci. 2021;86:4026–4036) Allicin inclusions with a-cyclodextrin effectively masking its odor: Preparation, characterization, and olfactory and gustatory evaluation (Zhou, Yong, et al) discloses Allicin, a chemical found in functional foods, has a variety of beneficial bioactivities but the unpleasent odor and unstability hinder its applications. Isolating products from cyclodextrin (CD) complexation, using ß-CD and its derivatives, is usually a time and energy-consuming process. Herein, a high-efficiency and eco-friendly preparation method of an inclusion (allicin@a-CD) formed by allicin and a-CD was designed, which turned liquid allicin into crystal particles with high-speed stirring (10,000 r/min) at 25°C for 10 min in water. In vivo and in vitro masking evaluations showed that the inclusion particles could decrease the unpleasant odor of allicin.

Pharmaceutics, Developments in Taste-Masking Techniques for Traditional Chinese Medicines (Zheng, Xiao, et al.) discloses several proteins (such as ß-lactoglobulin and ß-casein) could be covalently linked with some TCM-derived ingredients (e.g., EGCG, allicin, and quinine) with the purpose of modifying their unpleasant taste or odor.

Molecules, Review of Applications of Cyclodextrins as Taste-Masking Excipients for Pharmaceutical Purposes () discloses methods of evaluation of the taste-masking properties and the factors affecting the outcomes, such as the choice of the proper cyclodextrin or guest–host molar ratio. The conclusions of this review reveal that the application of CDs is not straightforward; nevertheless, this solution can be an effective, safe, and inexpensive method of taste masking for pharmaceutical purposes

OBJECTIVE OF INVENTION
Nowadays the trend of nutraceuticals with botanical ingredients is developing. Allicin is a phytochemical having a variety of beneficial bioactivities but the unpleasant odor and instability hinder its applications. Taste is one of the most important parameters governing patient compliance. Allicin having an undesirable taste and odor is one of several important formulation problems that are encountered with certain drugs. Taste masking and odor masking related to Allicin can avoid such type of drawbacks and can improve the rate of consumption of allicin-containing medications. It will contribute greatly to improving the compliance of consumers and provide a new and effective approach to broaden the application of allicin. To solve the above problem our invention provides a method to effectively mask the smell and taste.

SUMMARY OF THE INVENTION
The present invention belongs to the field of nutraceuticals and is specifically related to the taste masking of Allicin and the process thereof. In particular the present disclosure provides an allicin taste masking composition and preparation method thereof.
Further invention relates to allicin taste masking nutraceutical composition comprising various complexes such as ion exchange resin, beta cyclodextrins, and synergistic forms of Guar gum and Shilajit (Fulvic acid). Another invention belongs to ion exchange resin and beta cyclodextrins methods use chemical constituents, while synergistic forms of Guar gum and shilajit are natural phytoconstituents.
All three methods are evaluated and we concluded that the processing time, bioavailability and taste masking effects are better using the natural phyto constituent than using a chemical mixture. Allicin: Guar gum: Shilajit (Fulvic acid) complexes are evaluated for their structural characteristics by XRPD and DSC.

The evaluation of taste masking and odor masking are done using in vitro such as the dissolution method and in vivo techniques such as the determination of bitterness threshold concentration. Micromalatic properties of Guar gum: Shilajit complex with Allicin is also evaluated and found satisfactory. The mixture ratio amount of additives in Allicin: Guar gum: Shilajit is lower than chemical complexes.

BRIEF DESCRIPTION OF THE DRAWINGS
The following figures are illustrative of particular examples for method of the present disclosure, are descriptive of some of the embodiments and are not intended to limit the scope of the disclosure. The figures are not to scale (unless so stated) and are intended for use in conjunction with the explanations in the following detailed description.

Fig. 1 Phase solubility diagram
Fig. 2 Calibration curve for Allicin in distilled water
Fig. 3 Calibration curve for Allicin in 0.1 N HCL
Fig. 4 Calibration curve for Allicin in phosphate buffer of pH 6.8
Fig. 5: X- ray powder diffraction of A- Allicin, B- Guar gum: Shilajit, C- Allicin – Complex
Fig.6: In vitro Allicin release from Indion 234-Allicin resinate (n=5)
Fig. 7 Phase solubility diagram for Allicin-ß-CD system
Fig. 8 Allicin release in simulated intestinal fluid

DETAILED DESCRIPTION OF THE INVENTION
Detailed Description of the Invention While this specification concludes with claims particularly pointing out and distinctly claiming that, which is regarded as the invention, it is anticipated that the invention can be more readily understood through reading the following detailed description of the invention and study of the included examples.
The following is a detailed description of embodiments of the present disclosure. The embodiments are in such detail as to clearly communicate the disclosure. However, the amount of detail offered is not intended to limit the anticipated variations of embodiments; on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the present disclosure as defined by the appended claims.

Unless the context requires otherwise, throughout the specification which follow, the word “comprise” and variations thereof, such as, “comprises” and “comprising” are to be construed in an open, inclusive sense that is as “including, but not limited to.”

Reference throughout this specification to “one embodiment” or “an embodiment” means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrases “in one embodiment” or “in an embodiment” in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.

The headings and abstract of the invention provided herein are for convenience only and do not interpret the scope or meaning of the embodiments.
Various terms are used herein. To the extent a term used in a claim is not defined below, it should be given the broadest definition persons in the pertinent art have given that term as reflected in printed publications and issued patents at the time of.
In order to achieve the above technical objective, the technical solution adopted by the invention is described below.
The Allicin is estimated spectrophotometrically at 248.6 nm using JASCO-V520 -UV VIS spectrophotometer over a 2-12 µg/ml concentration range.

Preparation method of allicin taste masking complex using Ion exchange resin:
The resin that showed the highest loading efficiency is optimized for the Allicin: resin ratio and its loading efficiency is further checked to find optimum pH conditions for Allicin loading.

Preparation of Allicin resin complexes using batch process: An accurately weighed amount of Allicin (100 mg) is taken and dissolved in 100 ml distilled water. Then known weight (100mg) of ion exchange resin is added to the solution and stirred on the magnetic stirrer. The time to reach equilibrium is determined by periodically measuring the concentration of the Allicin solution. It is found that 5 hours is the optimum period for the attainment of loading equilibrium. Resinate thus formed is filtered and ished with an excess amount of deionized water. The Allicin content in the final filtrate is analyzed by UV-spectroscopy. Resinates are dried overnight in a hot air oven at 500C and then stored in tightly closed in desiccators.

Selection of Allicin resin ratio: Three batches are prepared to contain Allicin-resin in the ratio of 1:0.5, 1:1, and 1:1.5 with Indion 234 and with Indion 204 & 264. The pH of the solution is maintained at pH 6.0. The slurry is stirred for 2 hours. Resinates obtained are separated by filtration, ished with a copious quantity of deionized water and Allicin contents are determined.

Allicin Loading: For the Allicin loading batch method is used. allicin solution of concentration 1mg/ml is prepared in deionized water. The required quantity of resin is placed in an allicin solution and stirred till the attainment of equilibrium. The time for attainment of equilibrium is decided to be 6 hr from preliminary experimentation. The slurry is filtered and the amount of Allicin remaining in the filtrate is determined spectrophotometrically. The amount of Allicin adsorbed is determined by the difference between the amount of Allicin present in the stock solution and the amount remaining in the filtrate at the end of equilibrium.

Evaluation of Resinates:
Determination of Allicin content: Resinate (10mg) is placed in 1M HCl and stirred at 100 rpm for one hour. The solution is filtered and analyzed for the content of allicin. The Stability of complexes is determined by placing the weighed quantity of complex in deionized water for 24 hours and analyzed for Allicin content.

• Taste evaluation
The evaluation of taste is done in two parts.

a) Determination of threshold bitterness concentration: -
Various concentrations (1-30mcg /ml) of Allicin are prepared in phosphate buffer pH 6.7. The mouth is rinsed with this solution and then, l0 ml of the most dilute solution is tasted by swirling it in the mouth mainly near the base of the tongue for 30 seconds. If the bitter sensation is no longer felt in the mouth after 30 seconds, the solution is spat out and waited for 1 minute to ascertain whether this is due to delayed sensitivity. Then rinse with safe drinking water. The next highest concentration should not be tasted until at least 10 minutes have passed. The threshold bitter concentration is the lowest concentration at which a material continues to provoke a bitter sensation after 30 seconds. After the first series of tests, rinse the mouth thoroughly with safe drinking water until no bitter sensation remained. Wait for at least 10 minutes before carrying out the second test.

b) In-vitro evaluation of bitter taste of resinates: An accurately weighed (10 mg equivalent) resinate and 10 ml of pH 6.7 phosphate buffer (0.1 M) is taken in a series of volumetric flasks and stirred at 50 rpm. The stirring is stopped at different time intervals such as 0,10, 30,60 and 120 sec., the dispersion is filtered, and the concentration of Allicin in filtered resinate is determined. Time for resinate to achieve Allicin concentration corresponding to threshold bitterness in 10 ml phosphate buffer is recorded.

• Odor evaluation
The evaluation of odor is done by determination of odor threshold concentration:
Various concentrations of allicin complexes (1-30mcg /ml) of Allicin are prepared in phosphate buffer pH 6.7. Tips of absorbent perfumer paper strips are dipped into vials containing different allicin complex dilutions and numbered in ascending order. Total 7 Healthy volunteers without any olfactory complaints are recruited for odor testing. The volunteers are told not to eat, drink or chew gum before 1.5 hr. of testing. All the volunteers smelled dipped paper strips by placing strips under their noses. All the volunteers are allowed to sniff two to three times for 30 to 60 sec followed by 2 min intervals before smelling other strips with different dilutions. The concentration at which the volunteer sensed the smell is used to define the detection threshold.

Micromeritic property:
1. Angle of repose: Angle of repose has been defined as the maximum angle possible between the surface of the pile of powder the and horizontal plane. The angle of repose for the granules of each formulation is determined by the funnel method. The granule mass is allowed to flow out of the funnel orifice on a plane of paper kept on the horizontal surface. This forms a pile of the angle of granules on the paper. The angle of repose is calculated by substituting the values of the base radius ‘R’ and pile height ‘H’ in the following equation:
Tan ? = H / R
Therefore; ? = tan –1 (H / R)

2. Bulk density:
Table 1: Relationship between Angle of repose (?) and flowability
Angle of repose (?) Flowability
< 20 Excellent
20-30 Good
30-34 Passable
> 40 Very poor

Both loose bulk density (LBD) and tapped bulk density (TBD) are determined. A quantity of 20gm of powder from each formula is lightly shaken to break any agglomerates if any and then is introduced into a 50 ml measuring cylinder. It is allowed to fall under its own weight onto a hard surface from the height of 2.5cm at 2- second intervals. The tapping is continued until no further change in volume is noted. Loose bulk density (LBD) and Tapped bulk density (TBD) are calculated using the following formulae:
LBD = Weight of the powder/Volume of the packing
TBD = Weight of the powder/Tapped volume of the packing

3. Compressibility index: -
The compressibility index of the formulation blends is determined using Carr’s compressibility index:
Carr’s compressibility index (%) = [(TBD-LBD) X 100]/TB

Table 2: Relationship between % compressibility and flowability
% Compressibility Flowability
5-15 Excellent
12-16 Good
18-21 Fair passable
23-35 Poor
33-38 Very poor
<40 Very very poor.

Characteristics of Allicin resinates preparation: -

X-ray diffraction: X-ray diffraction patterns for Allicin, Natural blend and physical mixture of Allicin are obtained on Phillips analytical x-ray BV (PW1710) using cu anode, 40 kv voltage and current of 30 mA.
IR diffraction: The Infra red spectra of Allicin, Natural blend and physical mixture of Allicin are obtained using Fourier transform infrared (FTIR) spectroscopy (Jasco 460 plus, Tokyo, Japan) spectra are observed over wave number 4000 to 400 cm –1
DSC Study: Universal V4.1d TA differential scanning calorimeter is used to analyze the thermal behavior of Allicin, Natural blend and physical mixture of Allicin. Indium standard is used to calibrate the DSC temperature. The samples are heated at 10 OC per minute.

In-vitro Allicin release profile: In-vitro dissolution testing is an important tool in proper control and evaluations of Allicin from complex or resinate preparations various methods have been described in the literature. Despite attempts to develop standard methods, no such dissolution procedure has yet been accepted.
The following conditions mentioned in Table 3 are employed to study the in-vitro dissolution of Allicin- resin complex (resinate) preparations

Table 3: Conditions mentioned employed to study the in-vitro dissolution
USP Dissolution Apparatus Type II
Volume of Dissolution medium 900 ml
Speed of paddle rotation 100 rpm
Temperature 37 Deg C ± 0.5 Deg C
Dissolution Medium 0.1 N HCl
Test time 35 min
Sample size Allicin complex equivalent to 10 mg of Allicin
At 5 min. interval aliquots of medium (10ml) are taken, filtered and absorbance is measured by UV spectroscopy at 248.6 nm. The medium is replaced with an equal volume of fresh dissolution fluid.

Inclusion complex with B-Cyclodextrins
Determination of stability constant (K):
Complexation studies are performed according to the method reported by Higuchi. An excess amount of Allicin is added to the aqueous solutions of various concentrations (0.02-0.002 mM/L) of ß-CD solution (molecular weight = 1135). The contents are stirred for 72 hours at 37°C ± 1°C. After equilibrium, the samples are filtered and absorbance is measured at 248 nm (Jasco UV/Vis spectrophotometer, Japan). The apparent stability constant is calculated from the initial straight portion of the phase solubility diagram (Fig.1) using the following equation.

K 1: 1 = Slope/intercept (1 - slope)
K = 172.6 ML-1

Preparation of Inclusion Complexes: The complexes are prepared in 1:1 molar ratio by following methods
Spray drying method: Allicin and ß-CD are dissolved in ethanol and the mixture is stirred at 100 rpm for 3 hours after spray drying the complex. The inlet temperature is 800C & outlet temperature is 600C.
Kneading method: Allicin is added to the paste of ß-CD and the mixture is levigated for 45 min. The paste is dried at 50C and the dried mass is pulverized and sieved through # 100 meshes.

Inclusion complex with Guar gum and Shilajit (Fulvic acid)
The complexes are prepared in various molar ratios by following methods
Spray drying method: Allicin, Guar gum and Shilajit are dissolved in distilled water and the mixture is stirred at 100 rpm for 3-4 hours after spray drying the complex. The inlet temperature is 800C & outlet temperature is 600C.
Kneading method: Allicin is added to the paste of Guar gum and Shilajit and the mixture is levigated for 45 min. The paste is dried at 50C and the dried mass is pulverized and sieved through # 100 meshes.
Calibration curve for Allicin in distilled water: -
1. Standard stock solution: About 100 mg Allicin is accurately weighed and transferred to 100 ml volumetric flask. It is dissolved in distilled water and volume is made up to 100 ml.
2. Working stock solution: A series of Allicin solution ranging from 2 to 12 ?g/ml is prepared from standard stock solution. Spectra are run and the ?max is recorded.
The absorbance of all solutions is measured against blank at ?max.
Calibration curve for Allicin in 0.1 N HCl
Preparation of 0.1 N HCl: 8.5 ml of concentrated hydrochloric acid is added in distilled water and volume is adjusted up to 1000 ml by distilled water and mixed well.
1. Standard stock solution: About 100 mg Allicin is accurately weighed and transferred to 100 ml volumetric flask. It is dissolved in 0.1 N HCl and vothe lume is made up to 100 ml.
2. Working stock solution: A series of Allicin solutions ranging from 2 to 12 ?g/ml is prepared from the standard stock solution. Spectra are run and the ?max is recorded. The absorbance of all solutions is measured.

Calibration curve for Allicin in phosphate buffer of pH 6.8
Preparation of pH 6.8 (0.1 M) phosphate buffer: 27.2 mg of Potassium dehydrogenase phosphate is dissolved in 250 ml distilled water, mixed and added 112 ml of 0.2 M sodium hydroxide; volume is adjusted with water to 1 lit. And mixed well.52
A. Standard stock solution: About 100 mg of Allicin is accurately weighed and transferred to 100 ml volumetric flask. It is dissolved in pH 6.8 buffer solution and volume is made up to 100 ml.
B. Working stock solution: A series of the Allicin sol
C. Solution ranging from 2 to 12 µg/ml is prepared from standard stock solution. The spectra are run and ?max is observed. Absorbance of all solutions is measured.
Physical complex with Guar gum: Shilajit (Fulvic acid)
Table 4: Selection of Allicin: Guar gum: Shilajit
Complex
Allicin: Guar gum: Shilajit ratio % Allicin content in Physical mixer
Allicin: Guar gum: Shilajit 1: 0.2:0.2 37.57 ± 0.4791
1: 0.3:0.3 46.60 ± 0.3660
1: 0.4:0.4 42.88 ± 0.3223
Allicin: Guar gum: Shilajit (1: 0.3:0.3) gives best % of Allicin as compared other concentration of Allicin: Guar gum: Shilajit
Taste evaluation
Determination of threshold bitterness concentration
Most volunteers reported the threshold bitterness at 20 µg/ml.
Volunteers 1 2 3 4 5
6 7
Threshold bitterness conce µg/ml 20 10 20 20 20 20 20
Table 5: Threshold bitterness concentration

Time for the attainment of threshold bitterness concentration invitro
The time for this threshold bitterness concentration to be achieved in buffer of salivary pH showed that the Allicin is not released in saliva to attain threshold bitterness concentrations thereby masking the bitter taste satisfactorily
Table 6: Time for attainment of threshold bitterness concentration invitro
Stirring time sec 0 5 10 30 60 120
concentration (µg/ml) 1.15± 0.102 1.15± 0.128 1.5± 0.236 1.65± 0.162 1.85± 0.239 2.62± 0.124

Odor evaluation:
Odor threshold concentration is reported 30 µg/ml
Volunteers 1 2 3 4 5
6 7
Threshold Odor conc µg/ml 20 30 30 25 30 30 30
Table 7: Determination of Odor Threshold Concentration

Micromeritic properties
Further the micromeritic properties are evaluated using properties such as bulk density, angle of repose and compressibility (Carr) index are calculated in table. It is found that micromeritics property of Guar gum: Shilajit complex with Allicin is satisfactory than pure form of Allicin.
Table 8: Micromeritic properties of Allicin & Complex
Property Allicin Complex
Carr index
Bulk density
Angle of repose 18.46 %
0.3122 g/ml
28.89 20.12 %
0.421 g/ml
30.29
Each reading is a mean of three determinations.
XRPD study
The complexation is confirmed by carrying out X-ray powder diffraction study on Guar gum: Shilajit, Allicin and Complex. Allicin is Amorphous in nature while Guar gum: Shilajit is also amorphous. The molecular state of the Allicin in complex shows Sharp peak and the absence of Allicin peaks. This confirms that the entrapped Allicin is dispersed monomolecularly in the complex form. The difference in peaks obtained at various different ? values reveals that the samples are different from each other.
Inclusion Complex with ß-Cyclodextrin
Determination of stability constant (K)
Phase solubility diagram for Allicin-ß-CD system in water is shown in Figure 7. A linear increase in solubility of Allicin is observed with increasing concentration of ß-CD. Since the slope of the diagram is less than 1 (0.1107), the complex stoichiometry is assumed to be 1:1.
Phase solubility study.
K 1: 1 = Slope / intercept (1 - slope)
K = 103.6 ML-1

Preparation of Inclusion Complexes:
The complexes are prepared in 1:1 molar ratio by following methods
1) Spray drying method (SPR)
2) Kneading method (KN)
Taste evaluation
The taste evaluation is done in two parts; first the bitterness threshold concentration is determined using known concentrations of Allicin, which is found to be 20 µg/ml. The Allicin release from these complexes in simulated salivary fluid required 30 sec and 2 min to achieve threshold bitterness concentration for SPR and KN products respectively.

Table 9: Determination of threshold bitterness concentration
Volunteers 1 2 3 4 5
6 7
Threshold bitterness conc. (µg/ml) 25 20 20 25 20 25 20

In Vitro Dissolution Rate Studies
Further the Allicin release in simulated intestinal fluid showed from KN (92.42 % at 25 min) to be less than SPR complex (100 % at 25 min) (Figure 8). Thus, Allicin forms 1:1 stoichiometric complex with ß- cyclodextrin. The complexes are stable and can effectively mask bitter taste of the Allicin providing good in vitro release.

Odor evaluation:
Odor threshold concentration is reported 25 µg/ml
Volunteers 1 2 3 4 5
6 7
Threshold Odor conc µg/ml 25 25 30 25 25 30 25
Table 10: Determination of Odor Threshold Concentration

Ion exchange resin
Selection of Resin
Selection of resin for a specific application requires consideration of no. of features. Depending on the acidic & basic nature of the Allicin cationic and anionic exchange resin are used. In the presence work weak cation exchange resin resins i.e. Indion 204, Indion 234 & Indion 264 are used for the taste masking of Allicin. Weak cationic exchange resins are used here because of their weak binding capacity and basic nature of Allicin.
Table 11: Selection of Resin
Resin Allicin: resin ratio % Allicin content of resinate
Indion 204 1: 1 37.57 ± 0.4791
Indion 234 1: 1 46.60 ± 0.3660
Indion 264 1: 1 42.88 ± 0.3223

1) Indion 234 gives best loading achievement is 90 % at 5 h
2) Amount of Allicin present in the resinate is 46.60 % in (1:1) Allicin: Indion 234
Effect of Allicin: resin ratio on loading
Indion 234 gives best loading achievement is 90 % at 5 h. so Indion 234 selected for the further loading process for the taste masking. Different (Allicin: Indion-234) ratio such as 1:0.5, 1:1, 1:1.5, 1:2 is subjected to loading.
Allicin: Indion-234 (1: 1.5) ratio gives best loading is 91 %, as well as more amount of the Allicin present in resinate is 47.85
Table 12: Effect of Allicin: resin ratio on loading
Resin Allicin: Resin ratio % Allicin content of resinate
Indion 234 1:0.5 41.20± 0.4083
1:1 46.77± 0.3885
1:1.5 47.85 ± 0.1836
1:2 47.73 ± 0.2405

Taste evaluation
Determination of threshold bitterness concentration
Most volunteers reported the threshold bitterness at 20 µg/ml.
Volunteers 1 2 3 4 5
6 7
Threshold bitterness conce µg/ml 20 10 20 20 20 20 20
Table 13: Determination of threshold bitterness concentration

Time for attainment of threshold bitterness concentration
The time for this threshold bitterness concentration to be achieved in buffer of salivary pH showed that the Allicin is not released in saliva to attain threshold bitterness concentrations thereby masking the bitter taste satisfactorily
Table 14: Time for attainment of threshold bitterness concentration invitro
Stirring time sec 0 5 10 30 60 120
concentration (µg/ml) 1.25± 0.124 1.45± 0.2587 1.57± 0.2478 1.91± 0.1569 3.75± 0.1782 6.62± 0.2247

Odor evaluation:
Odor threshold concentration is reported 30 µg/ml
Volunteers 1 2 3 4 5
6 7
Threshold Odor conc µg/ml 25 30 30 25 30 30 30
Table 15: Determination of Odor Threshold Concentration

Micromeritic properties
Further, the micromeritic properties are evaluated & are calculated in table 16. It is found that all the properties of resin and resinate are similar.
Table 16: Micromeritic properties
Property Allicin Resinate
Carr index
Bulk density
Angle of repose 18.46 %
0.3122 g/ml
28.89 19.12 %
0.327 g/ml
29.24

,CLAIMS:1. An allicin taste masking nutraceutical composition and the process thereof.
2. The allicin taste masking nutraceutical composition as claimed in claim 1, wherein the allicin taste masking nutraceutical composition comprising various complexes such as ion exchange resin, beta cyclodextrins, and synergistic forms of Guar gum and Shilajit (Fulvic acid).
3. The allicin taste masking nutraceutical composition as claimed in claim 1, wherein the nutraceutical composition belongs to ion exchange resin and beta cyclodextrins methods use chemical constituents, while synergistic forms of Guar gum and shilajit are natural phytoconstituents.
A method of preparation of allicin taste masking complex using Ion exchange resin comprises of;
a. Preparation of Allicin resin complexes using batch process
b. Selection of Allicin resin ratio
c. Allicin Loading batch method
4. The allicin taste masking nutraceutical composition as claimed in claim 1, wherein Allicin: Guar gum: Shilajit (Fulvic acid) complexes are evaluated for their structural characteristics & it confirms that the entrapment of Allicin is dispersed monomolecularly in the complex form.
5. The allicin taste masking nutraceutical composition as claimed in claim 1, wherein the evaluation of taste masking and odor masking are done using in vitro such as the dissolution method and in vivo techniques such as the determination of bitterness threshold concentration.
6. The allicin taste masking nutraceutical composition as claimed in claim 1, wherein the Micromalatic properties such as angle of repose, bulk density, compressibility index of Guar gum: Shilajit complex with Allicin is also evaluated.

Documents

Application Documents

# Name Date
1 202321026173-STATEMENT OF UNDERTAKING (FORM 3) [07-04-2023(online)].pdf 2023-04-07
2 202321026173-PROVISIONAL SPECIFICATION [07-04-2023(online)].pdf 2023-04-07
3 202321026173-FORM FOR SMALL ENTITY(FORM-28) [07-04-2023(online)].pdf 2023-04-07
4 202321026173-FORM FOR SMALL ENTITY [07-04-2023(online)].pdf 2023-04-07
5 202321026173-FORM 1 [07-04-2023(online)].pdf 2023-04-07
6 202321026173-EVIDENCE FOR REGISTRATION UNDER SSI(FORM-28) [07-04-2023(online)].pdf 2023-04-07
7 202321026173-EVIDENCE FOR REGISTRATION UNDER SSI [07-04-2023(online)].pdf 2023-04-07
8 202321026173-DRAWINGS [07-04-2023(online)].pdf 2023-04-07
9 202321026173-DECLARATION OF INVENTORSHIP (FORM 5) [07-04-2023(online)].pdf 2023-04-07
10 202321026173-FORM 3 [06-04-2024(online)].pdf 2024-04-06
11 202321026173-ENDORSEMENT BY INVENTORS [06-04-2024(online)].pdf 2024-04-06
12 202321026173-DRAWING [06-04-2024(online)].pdf 2024-04-06
13 202321026173-CORRESPONDENCE-OTHERS [06-04-2024(online)].pdf 2024-04-06
14 202321026173-COMPLETE SPECIFICATION [06-04-2024(online)].pdf 2024-04-06
15 202321026173-FORM-26 [16-07-2024(online)].pdf 2024-07-16
16 202321026173-FORM 3 [08-01-2025(online)].pdf 2025-01-08
17 202321026173-FORM 18 [22-02-2025(online)].pdf 2025-02-22