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Mineral Enriched Compositions And Process For Preparing The Same

Abstract: The present invention relates to a calcium enriched composition having high calcium content wherein free calcium is present in between the range of 41- 44 % w/w and a process for its preparation from natural sources like shells, conchs etc. The natural calcium composition comprises of calcium citrate present in between the range of 25- 26 % w/w, calcium ascorbate present in between the range of 0.1- 0.13 % w/w and calcium carbonate present in between the range of 74-75 % w/w.

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Patent Information

Application #
Filing Date
18 March 2013
Publication Number
50/2014
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application

Applicants

DABUR INDIA LIMITED,
8/3 ASAF ALI ROAD, NEW DELHI-110002, INDIA

Inventors

1. J.L.N. SASTRY
DABUR RESEARCH & DEVELOPMENT CENTRE, NO. 22, SITE IV, SAHIBABAD-201010, GHAZIBAD, UTTAR PRADESH
2. RAJEEVA KUMAR RAI
DABUR RESEARCH & DEVELOPMENT CENTRE, NO. 22, SITE IV, SAHIBABAD-201010, GHAZIBAD, UTTAR PRADESH

Specification

Field of the Invention
The present invention relates to a natural calcium composition and a process for
preparing the same. The present invention, in particular, relates to calcium enriched
natural compositions obtained from natural sources through a novel process.
Background of the Invention
Calcium serves two important functions in the body - the building of bones and teeth
and regulating certain body processes. Once the bone is formed, it continues to
change with the processes of building new bone and maintaining the old. The normal
behavior of heart muscles, nerves and the blood clotting processes all depend on the
presence of calcium.
Calcium is essential for living organisms, in particular in cell physiology, where
movement of the calcium ion Ca2
+ into and out of the cytoplasm functions as a signal
for many cellular processes. As a major material used in mineralization of bone, teeth
and shells, calcium is the most abundant metal by mass in many animals. The body
contains more calcium than any other mineral. Calcium plays an important role in
building stronger, denser bones early in life and keeping bones strong and healthy
later in life. Ninety-nine percent of the total calcium in the body is concentrated in the
bones and teeth; the remainder is in the fluids and soft tissues. The mineral calcium is
vitally important to support tissue, bones and cells in the body. Calcium aids in the
activation of enzymes for proper digestion and encourages a healthy heart and
nervous system.
Calcium together with other mineral elements gives rigidity and permanence to bones
and teeth. These characteristics make it possible for the bone to be support of the
body, providing the rigid structure to which the muscle tissue is attached. Bones
forms protective cavities for vital organs - the heart and lungs in the chest cavity, the
brain in the cranial cavity. Bone will with stand almost as much weight as cast iron
before breaking. It is itselflight in weight.
The calcium absorbed combines with phosphorus and water to form calcium
phosphate. First fibrous network made up of collagen and other nitrogenous
substances is formed. Then the bone minerals are deposited on this network as
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crystals. These crystals are re-dissolved and recrystallized to form bone tissue. During
recrystallization some of the water is lost and the structure of crystals is also changed
to form bone.
A number of factors influence the mineralization and resorption of bone. Amount of
vitamin D at the bone site is essential for the deposit of minerals in to the matrix. On
the other hand, the activities of the parathyroid gland bring about resorption of bone.
The emotions have an important bearing up on the calcium balance.
Calcium requirements vary throughout the life of a living organism according to age,
stress, medical conditions, allergies and disease. However, a significant portion of the
population fails to achieve the daily-recommended 1,000 to 1,200 mg of calcium.
Calcium is available through many sources. The best natural sources are milk, milk
products (cheese, curd, skimmed milk, butter milk etc.), egg yolk and fish. The
cheapest dietary sources are green leafy vegetables, but calcium is in insoluble form
so it cannot be absorbed properly. Calcium is also found in drinking water and in
some fruits. A balanced diet including dairy products, broccoli, spinach, legumes and
other calcium-rich foods are the best sources.
If calcium is taken in low quantities or if it does not meet the body requirements,
rickets and osteomalacia can arise. In rickets, the bones are bent at the ankles.
Calcium deficiency can cause abnormal formation of bones. Such abnormalities can
lead to problems during pregnancy and delivering babies. In order to prevent birth
' defects and complicated pregnancies, pregnant women should eat a calcium-rich diet
and consume dietary supplements after consultation with a doctor to fulfil their daily
calcium requirements. After 50 years of age, calcium deficiency can lead to decrease
in the bone density, and this can lead to easy fractures. It is generally recommended
that postmenopausal women should consume up to 1500 mg of calcium coming from
both dietary sources and calcium supplements.
Deficiency of calcium can cause symptoms such as mood swings, headaches, kidney
stones, numbness or muscle cramping, increased cholesterol levels and bone
deterioration.
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In order to meet the daily-recommended amount of calcium, there is a need for intake
of calcium supplements.
Calcium carbonate is the most widely used compound in making calcium supplements
because it is abundantly available as natural sources, and therefore it is inexpensive. A
variant of calcium carbonate known as coral calcium is also used in making effective
calcium tablets and liquid supplements. However, some side effects are still possible
like indigestion, constipation, diarrhoea, headache and infections. In any case, one
should not consume more than 2500 mg of calcium per day.
Calcium citrate is the salt that comes from citrus juice concentrates such as orange,
lime, lemon or grapefruit, and it can also come directly from the fruit. Calcium citrate
is a calcium supplement, which is used to treat a variety of conditions related to the
bones such as osteoporosis. Along with other minerals supplements such as zinc
picolinate, magnesium glycinate, and manganese, calcium citrate can support healthy
immune function and is used to treat immune-related conditions such as chronic
fatigue syndrome.
Calcium citrate is a compound employed in the making of effective calcium tablets. It
is easily absorbed by the blood stream, and therefore can be consumed before meals.
However, unlike calcium carbonate, calcium citrate does not provide a lot of
elemental calcium which is useful for the blood.
While calcium citrate is an acidic form of calcium, calcium carbonate, another
calcium supplement, is alkaline in nature. Both supplements can provide calcium for
the body's use, though there are differences. As an acid-based supplement, calcium
citrate can be taken at any time of day, whereas calcium carbonate must be taken after
a meal or with an acidic beverage like orange juice. However, calcium citrate pills
contain less elemental calcium than calcium carbonate pills, and therefore must be
taken in greater quantities to receive the same amount of calcium.
Calcium carbonate provides up to 40% of elemental calcium. This means that if a
tablet contains 1000 mg of calcium carbonate, it provides 400 mg of elemental
calcium which is absorbed by the blood stream. But a 1000 mg source of calcium
citrate provides up to 300 to 350 mg of elemental calcium. It is recommended to
consume calcium citrate along with a calcium-rich diet and lots of fluids. Calcium
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absorption is greatly influenced by the food we eat. Healthy foods assist in calcium
absorption along with vitamin D and phosphorus, whereas sugar, tea, coffee, tobacco,
carbonated drinks and alcohol disturb calcium absorption.
Supplements made from calcium citrate are readily absorbed into the body because
they do not require extra stomach acid for absorption. As a result, the calcium goes to
work faster because calcium citrate has its own naturally acidic environment.
However, some people are allergic to source of calcium citrate. They are unable to
digest it and as a result the calcium consumed through calcium citrate supplements
goes out through urine. Such people are also at high risk of developing kidney stones.
Hence, there is a need to develop calcium enriched supplements which contain
maximum amount of calcium and which are obtained from natural sources so as to
reduce the side effects associated with known calcium supplements.
The present invention relates to a natural calcium composition having high calcium
content. Despite the large number of calcium compositions currently available and
known in the art, many of them are known have some side effects. Although calcium
carbonate based supplements are abundantly available from the natural sources and
are inexpensive, the side effects like digestion, constipation, diarrhea, headache and
infections are known. People prone to calcium citrate allergies are unable to digest
such a composition and as a result the calcium consumed through calcium citrate
supplements goes out through urine. Such people are at high risk of developing
kidney stones.
The natural calcium composition of the present invention aims to mitigate the risks
associated with the known calcium compositions and provides high calcium content.
This natural calcium composition was obtained from natural sources and specifically
from the natural sources like shells, conchs etc. These natural sources are processed in
lime juice through calcinations.
Summary of the invention:
According to an embodiment of the invention there is provided a natural calcium
composition having high calcium content.
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According to an embodiment of the invention there is provided a natural calcium
composition obtained from natural sources like shells, conchs etc.
In accordance with another embodiment of the invention there is provided a natural
calcium composition having free calcium present in between the range of 41- 44 %
w/w.
According to another embodiment of the invention there is provided a natural calcium
composition having free calcium present preferably in between the range of 41.5- 43.2
%w/w.
According to yet another embodiment of the invention there is provided a natural
calcium composition comprising calcium citrate present in between the range of 25-
26 % w/w, calcium ascorbate present in between the range of 0.1- 0.13 % w/w and
calcium carbonate present in between the range of74- 75% w/w.
According to another embodiment of the invention there is provided a natural calcium
composition comprising calcium citrate present preferably in between the range of
25.18-25.35% w/w, calcium ascorbate present preferably in between the range of
0.1075-0.1286% w/w and calcium carbonate present preferably in between the range
of74.54- 74.70% w/w.
According to yet another embodiment of the invention there is provided a process for
producing a natural calcium composition having high calcium content.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition obtained from natural sources like shells,
conchs etc.
According to an embodiment of the invention there is provided a process for
producing a natural calcium composition wherein the natural sources are processed in
lime juice through calcinations.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition comprising the steps:
1. Preparation of Shankh Bhasma
6
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2. Conversion of Shankh Bhasma into the natural calcium composition
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein said Shankh Bhasma is prepared
comprising the steps:
1. Cleaning of Shankh
2. Subjecting cleaned Shankh to Shankh Shodhana resulting in Shodhit Shankh
3. Incineration of the Shodhit Shankh by Shankh Marana resulting in Bhasma
Powder.
4. Converting the Bhasma Powder into finely powdered Shankh Bhasma.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein small Shankh pieces are cleaned by
washing with hot water and further bundled in the muslin cloth.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein said pieces of Shankh bundled in
muslin cloth are immersed and boiled for up to 3-6 hours into sufficient amount of
lemon juice.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein said pieces of Shankh bundled in
muslin cloth are immersed and boiled preferably for at least three hours into sufficient
' amount of lemon juice.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein lemon juice is in an amount of 1 :4
to 1:16
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein lemon juice is preferably in an
amount of 1 :8.
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According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein lemon juice is intermittently added
to maintain the immersion level of said pieces of Shankh bundled in muslin cloth.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein the Shodhit Shankh is placed into
clean earthen crucible and subjected to Gaja Puta incineration in Muffle Furnace for
4-8 hours at 700-800°C resulting in Bhasma Powder.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein said collected Bhasma Powder is
soaked in water overnight and allowed to dry in a hot air oven preferably at 60-70°C.
According to another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein said oven dried Bhasma Powder is
passed through #80 mesh S.S. sieve resulting in finely powdered Shankh Bhasma.
According to yet another embodiment of the invention there is provided a process for
producing a natural calcium composition wherein finely powdered Shankh Bhasma is
converted into natural calcium composition comprising the steps:
1. Soaking the Shankh Bhasma in sufficient amount of fresh lemon juice
to form a soaked bulk .
2. Agitating the soaked bulk of step 1 intermittently.
3. Drying the soaked bulk in a hot air oven at 40-50°C resulting in dried
bulk.
4. Passing the dried bulk of step 3 through #40 mesh S.S. sieve resulting
in the natural calcium composition.
The natural calcium composition of the present invention is in the form of fine
powder, granule, flake or any other suitable form and used as pharmaceutical
supplement, food and beverage additive etc.
Brief description of the drawings:
The invention can be described in the terms of the following figures whereFigure
1 a: Chromatogram for 50 mg/L Citrate Standard
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Figure 1 b: Chromatogram for determination of Calcium citrate for sample 27/170A
Figure 1 c: Chromatogram for determination of Calcium citrate for sample 27/170B
Figure 1d: Chromatogram for detennination of Calcium citrate for sample 27/170C
Figure 2a: Titration curve for standardization of0.01 mol/L ofCeric sulfate
Figure 2b: Titration curve for determination of Calcium ascorbate for sample 27/170A
Figure 2c: Titration curve for determination of Calcium ascorbate for sample 2 7/170B
Figure 2d: Titration curve for detennination of Calcium ascorbate for sample 27/170C
Detailed description of the invention:
Discussed below are some representative embodiments of the current invention. The
invention in its broader aspects is not limited to the specific details, representative
devices and methods, and illustrative examples shown are described in this section in
connection with the embodiments and methods. The invention according to its various
aspects is particularly pointed out and distinctly claimed in the attached claims read in
view of this specification, and appropriate equivalents.
It is to be noted that, as used in the specification and the appended claims, the singular
forms "a," "an," and "the" include plural referents unless the context clearly dictates
otherwise. Thus, for example, reference to a composition containing "a compound"
includes a mixture of two or more compounds. It should also be noted that the term
"or" is generally employed in its sense including "and/or" unless the content clearly
dictates otherwise.
The expression of quantity in terms of "% w/w" means the percentage by weight,
relative to the weight of the total solution or composition, unless otherwise specified.
The term "about," as used herein, modifying the quantity of an ingredient in the
compositions of the invention or employed in the methods of the invention refers to
variation in the numerical quantity that can occur, for example, through typical
measuring and liquid handling procedures used for making concentrates or use
solutions; through inadvertent error in these procedures; through differences in the
manufacture, source, or purity of the ingredients employed to make the compositions
or carry out the methods; and the like. The term about also encompasses amounts that
differ due to different equilibrium conditions for a composition resulting from a
particular initial mixture. Whether or not modified by the term "about," the claims
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include equivalents to the quantities. All numeric values are herein assumed to be
modified by the term "about," whether or not explicitly indicated. The term "about"
generally refers to a range of numbers that one of skill in the art would consider
equivalent to the recited value (i.e., having the same function or result). In many
instances, the terms "about" may include numbers that are rounded to the nearest
significant figure.
The natural calcium composition of present invention contains high calcium content
in free form.
The natural calcium composition of present invention has high calcium content. The
natural calcium composition of present invention comprises of calcium citrate,
calcium ascorbate and calcium carbonate and has high calcium content. This natural
calcium composition is obtained from natural sources and specifically from the
natural sources like shells, conchs etc. These natural sources are processed in lime
juice through calcinations. Most fruit juices contain organic acids which have
characteristics similar to those of lemon juice but none of said organic acids except
lemon juice have the efficacy to extract mineral compositions from the conch shells.
The free calcium is present in between the range of 41- 44 % w/w and more
preferably in between the range of 41.5- 43.2% w/w. The free calcium content of the
natural calcium composition of the present invention was determined by Inductively
Coupled Plasma Mass Spectrometry (ICP-MS) for the three samples Sample 27/170
A, Sample 271170 Band Sample 27/170 C. The details for the preparation of samples,
the instruments used, the experimental instrument conditions for ICP-MS and the
analysis are given in Example 1.
The natural calcium composition of present invention comprises calcium citrate which
is present in between the range of 25-26 % w/w and more preferably in between the
range of 25.18- 25.35% w/w. The amount of calcium citrate present in the natural
calcium composition of present invention is determined by using suppressed
conductivity detection. Metrosep A Supp 4 250/4.0 column is used with sodium
carbonate and sodium bicarbonate with sodium hydroxide as eluent for the three
samples Sample 27/170 A, Sample 27/170 B and Sample 27/170 C. The reagents,
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instruments, solutions used and the parameters maintained for this estimation are
provided in Example 2.
The natural calcium composition of present invention also compnses of calcium
ascorbate which is present in between the range of 0.1- 0.13 % w/w and more
preferably in between the range of 0.1075- 0.1286 % w/w. The amount of calcium
ascorbate present in the natural calcium composition of present invention is
determined by redox titration using Combined-Pt-ring electrode for the three samples
viz; Sample 27/170 A, Sample 271170 B and Sample 271170 C. The reagents,
instruments, solutions used and the parameters maintained for this estimation are
exemplified by Example 3.
The natural calcium composition of present invention also compnses of calcium
carbonate which is present in between the range of 74-75% and preferably present in
between the range of 74.54- 74.70% w/w. The amount of calcium carbonate was
determined by subtracting the amount of calcium citrate and calcium ascorbate from
the total mass of the natural calcium composition of present invention for three
samples i.e. Sample 27/170 A, Sample 27/170 B and Sample 271170 C. These
amounts are exemplified by Example 4.
The present invention is more particularly described in the following examples that
are intended as illustrations only, since numerous modifications and variations within
the scope of the present invention will be apparent to those of skill in the art. Unless
otherwise noted, all parts, percentages, and ratios reported in the following examples
are on a weight basis, and all reagents used in the examples were obtained or are
available from the chemical suppliers.
Three samples of the natural calcium composition were used viz; Sample 271170 A,
Sample 27/170 B and Sample 27/170 C. These samples were developed by utilizing
the process provided for producing a natural calcium composition.
Example 1
Analysis of free Calcium content in natural calcium composition
The free Calcium content in natural calcium composition was determined by
Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The instruments used for
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the analysis of Calcium content m natural calcium composition were Inductively
Coupled Plasma
Mass Spectrometer (ICP-MS) and Microwave Reaction System (MRS).
Sample Preparation:
6.0 ml of cone. HN03 was added to 0.1 g of sample and the resulting mixture was
digested as per the microwave reaction system program. The parameters of the
microwave reaction system program are provided in the Table 1. After digestion the
content ofvessel was transferred to a 100 ml volumetric flask and rinsed with Milli-Q
water. The rinsing was transferred to the volumetric flask and the required volume
was made up with water.
Table 1: Parameters of Microwave Reaction System Program used in ICP-MS.
Microwave Reaction System Program
Step Power (W) Ramp (min) Hold (min) Fan
1 600 5 15 1
2 800 5 10 1
3 0 - 10 3
Blank Solution Preparation:
6.0 ml nitric acid was taken in the sample vessel and digested in the same condition as
' for the sample solution preparation. Final volume of 100 ml was prepared with water.
The resulting solution was used as blank solution.
Preparation of working Standard:
Working standards of varying concentrations i.e. 100 ppm, 20 ppm, 15 ppm, 10 ppm,
5.0 ppm, 2.0 ppm, 1.0 ppm, 0.5 ppm were prepared by pipetting out required amounts
of Calcium Certified Reference Standard and making up the volume by using diluent
Analysis by ICP-MS:
ICP-MS plasma was optimized for 10-20 minutes. ICP-MS was calibrated using 0.5,
1.0, 2.0, 5.0, 10.0, 15.0 & 20 ppm working standards. The sample was analyzed by
diluting it 50 times using 1% HN03. The amounts of free calcium present in the three
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samples of natural calcium composition were determined and are tabulated in Table 2.
The mass of calcium analyte considered for the IPC-MS analysis was 44 and KED
(Kinetic Energy Discrimination) mode was utilized.
Table 2: The amount of Calcium ascorbate present in natural calcium
composition
Lot number Free calcium content (% w/w)
271170 A 41.5
27/170 B 41.9
271170 c 43.2
Example 2
Determination of Calcium Citrate in natural calcium composition
The calcium citrate content in natural calcium powder is determined by usmg
suppressed conductivity detection. Metrosep A Supp 4 250/4.0 column is used with
sodium carbonate and sodium bicarbonate with sodium hydroxide as eluent. The
samples, reagents, instruments, solutions used and the parameters maintained for this
estimation are given below.
Reagents:
Sodium carbonate (Fluka grade)
Sodium bicarbonate (Fluka grade)
Sodium hydroxide- 50-52% solution (Fluka grade)
Nitric acid (Merck GR)
Sulfuric acid (Merck GR)
Citric acid (Fluka grade)
Ultrapure water of resistivity> 18M O.cm (25°C), type I grade (ASTM D1193)
Solutions:
a) Eluent: 5.0 mml/L sodium carbonate and 3.0 mmol/L sodium bicarbonate and 1
mmol/L sodium hydroxide.
b) Regeneration solution: 1 00 mmol/L sulphuric acid
c) Rinsing solution: Ultrapure water
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d) Standard solutions: I OOOmg/L Citrate standard is prepared from Citric acid salt by
diluting with ultrapure water.
All the lower level standards of concentrations 50 mg/L, 100 mg/L, 150 mg/L and 200
mg/L were prepared from above I 00 mg/L standard by diluting with ultrapure water
Sample Preparation:
In a I 00 mL volumetric flask, 100 mg of the sample was dissolved into a solution of,
40 mL of water and 0.1 mL of cone. HN03. The solution was made up to the mark
using ultrapure water. This solution was sonicated and filtered through 0.2 flm filter
paper followed by IC-H cartridge and then injected in to the ion chromatograph.
' Various titrations parameters for the Metrosep A Supp 250/4.0 column in the
determination of Citrate in natural calcium composition are as indicated in Table 3.
Ultrapure water is injected as blank.
'
Table 3: Titration parameters for the Metrosep A Supp 250/4.0 column in the
determination of Citrate in natural calcium composition
Eluent Flow 1.0 mL!min
Sample volume 5 flL
Sampling Device 858 Autosampler
Recording time 20 minutes
Column temperature Ambient
Peristaltic pump on
MSM-11 Active
The amounts of Calcium Citrate present all the three samples of natural calcium
composition were calculated by using the Automatic integration with Magic Net 3.0
software using peak area for Citrate. These results are tabulated in Table 4.
Table 4: Amount of Calcium Citrate present in samples of natural calcium
composition
Lot number Calcium Citrate (in %)
27/I70 A 25.18
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27/170 B 25.18
27/170 c 25.35
The standard chromatogram and the chromatogram for the samples 27/170 A, 27/170
B and 27/170 C are indicated by the figures 1 a, 1 b, 1 c and 1 d respectively.
Example 3
Determination of Calcium ascorbate in natural calcium composition
Calcium ascorbate in calcium mineral is detennined by redox titration usmg
Combined-Pt-ring electrode. The samples, reagents, instruments, solutions used and
the parameters maintained for this estimation are given below.
' Reagents:
'
Ammonium Iron (II) sulfate (Merck GR)
Ceric sulphate (Merck GR)
Sulfuric acid (Merck GR)
Hydrochloric acid (Merck GR)
Solution Preparation:
Ceric sulphate titrant (0.01 mol/L) was prepared by dissolving 3.5 g of eerie sulphate
in 6 mL of 1:1 sulfuric acid/water mixture. This mixture was then gently warmed to
dissolve the salt completely. The resulting solution was cooled and diluted to 1000
mL in a volumetric flask.
Standardisation of Ceric sulphate:
0.05 g of Ammonium Iron (II) sulphate was dissolved in the mixture of 1 mL
concentrated sulphuric acid & 60 ml deionised water. This solution was titrated
against eerie sulphate using combined Pt-ring electrode till the first equivalence point.
Sample analysis:
0.5 g of sample was dissolved in 1 mL concentrated Hydrochloric acid sonicated for
20 sec. 60 mL distilled water was added and the content was titrated against Ceric
sulphate using combined Pt-ring electrode till the first equivalence point. The
titrations parameters for the combined Pt-ring electrode are as indicated in Table 5.
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Table 5: Titration parameters for the combined Pt-ring electrode in the
determination of Ascorbic acid in natural calcium composition
MetU
Signal Drift 50.0 mY/min
Min. Waiting time 10 s
Max. Waiting time 12 s
Volume increment 0.02 mL
Dosing rate Max mL/min
Start Conditions
Start Volume OmL
Pause 15 s
Stop Conditions
Stop volume 3mL
Stop measured value Off
Stop EP Off
Potentiometric evaluation
EP criterion 10mV
EP recognition Greatest
The amount of calcium ascorbate was calculated by using the following formula:
Calcium ascorbate(%)= Titer* EP* 215.12
SS*10*2
Where,
Titer= Actual strength of titrant (0.0101 mol/L)
EP = Titrant consumption for the first equivalence point in ml
SS =Sample size in g.
215.12= factor calculated as shown below
Factor 215.12 = [(molecular weight of calcium ascorbate - molecular weight of
calcium) /2] +molecular weight of calcium= [(390.31- 40.078)/2] + 40.078
The amounts of Calcium ascorbate present in all the three samples of natural calcium
composition obtained are tabulated in Table 6.
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Table 6: The amount of Calcium ascorbate present in natural calcium
composition
Sample ID (R.N o) Trial-1 (in %) Trial-2 (in %) Mean (in%)
27/170 A 0.1320 0.1252 0.1286
27/170 B 0.1184 0.1204 0.1194
27/170 c 0.1045 0.1105 0.1075
The titration curves for the standard and the samples 27/170 A, 27/170 Band 27/170
Care indicated by the figures 2a, 2b, 2c and 2d respectively.
Example 4
Determination of Calcium carbonate
The amount of calcium carbonate was determined by subtracting the amount of
calcium citrate and calcium ascorbate from the total mass of the composition and the
results are tabulated in Table 7.
Table 7: The amount of Calcium carbonate present in natural calcium
composition
Sample ID (R.No) Calcium Carbonate (in%)
27/170 A 74.69
27/170 B 74.70
27/170 c 74.54
The present invention is further directed to a process for producing a natural calcium
composition produced by converting finely powdered Shankh Bhasma into the natural
calcium composition. The Shankh Bhasma is a white colored, amorphous and water
insoluble powder prepared from the natural sources like shells, conchs etc. Large
pieces of Shankh are broken down into smaller pieces and deposits from the Shankh
pieces are removed by scrapping. After scrapping, Shankh pieces are cleaned by
washing properly with hot water. The clean Shankh pieces are bundled into a clean
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muslin cloth, immersed into lemon juice in an amount of 1 :4 to 1:16 and preferably
present in an amount of 1 :8. This mixture is boiled for 3-6 hours resulting in Shodhit
Shankh. Lemon juice is added intennittent1y to maintain the immersion level of the
Shankh pieces. The Shodhit Shankh is converted into fine powder and placed into
cleaned earthen crucible which is sealed with another inverted earthen crucible,
muslin cloth smeared with fuller's earth and further subjected to Gaja Puta
incineration in Muffle Furnace for 4-8 hours at 700-800°C. The Gaja Puta
incineration results in Bhasma Powder which is further fine powdered and soaked into
water for overnight. The water is decanted and settled down Bhasma Powder is
allowed to dry in a hot air oven at the 60-70°C. The dried bulk is through #80 mesh
S.S. sieve to get finely powdered Shankh Bhasma.
The finely powdered Shankh Bhasma hence obtained is converted into the natural
calcium composition by soaking 700 g Shankh Bhasma in sufficient amount of fresh
lemon juice (soaked bulk) in a S.S vessel. Soaked bulk is kept at room temperature for
three hours with intermittent agitation, spread in S.S. trays and dried in a hot air oven
at 40-50°C.The dried bulk is taken out from trays and passed through #40 mesh S.S.
sieve. 675-700 g of finely powdered natural calcium composition hence obtained is a
combination of the Calcium Citrate, Calcium Ascorbate and Calcium Carbonate.
It should be recognized that the preferred embodiment described above is exemplary
only. Certain modifications and improvements will occur to those skilled in the art
upon a reading of foregoing description. It should be understood that all such
modifications and improvements have been deleted herein for the sake of conciseness
and readability but are properly within the scope of the claims.
18
APPENDIX
Terminology used with their definitions:
1) Shankha: A conch shell of a species of large predatory sea snail, Turbinella pyrum
living in the Indian Ocean.
2) Shankha Bhasma: A traditional Ayurvedic preparation derived from the calcinated
conch shell of Turbinella pyrum
3) Slwdhana: Shodhana is an Ayurvedic purification process through which the
' external and internal impurities of metals and minerals are removed.
'
4) Shod hit Shankha: Purified conch shell.
5) Marana: Marana is essentially the burning process or calcination.
6) Puta: Specially designed fire-place for reducing the minerals to bhasma form.
These fire pl,aces are arranged in pits of different sizes dug in the earth depending
upon the heat requirement. The main purpose of the Puta is to cook the mineral with
the required quantity of heat constantly for a sufficient period.
7) Gaja Puta: The fire-place designed such that the pit is filled up with cow-dung
cakes till half of its capacity along in which the sealed crucible is kept. Then the
remaining portion of the pit filled up with more cow-dung cakes and ignited.

We Claim:
1. A natural calcium composition having high calcium content, wherein free calcium
is present in between the range of 41- 44 % obtained from calcium citrate, calcium
ascorbate and calcium carbonate.
2. The natural calcium composition as claimed in claim 1, wherein calcium citrate is
present in between the range of25-26% w/w.
3. The natural calcium composition as claimed in claim 1, wherein calcium
ascorbate is present in between the range of0.1- 0.13% w/w
4. The natural calcium composition as claimed in claim 1, wherein calcium
carbonate is present in between the range of74- 75% w/w.
5. The natural calcium composition as claimed in claim 1, wherein said natural
calcium composition is obtained from natural sources like shells, conchs etc.
6. A process for producing natural calcium composition as claimed m claim 1,
wherein the natural sources are processed in lime juice through calcinations.
7. The process as claimed in claim 6, wherein natural sources are selected from
shells, conchs etc.
8. The process as claimed in claims 6 to 7, wherein the process for producing a
natural calcium composition comprising the steps:
Preparation of Shankh Bhasma
Conversion of Shankh Bhasma into the natural calcium composition.
9. The process as claimed in claims 8, wherein the Shankh Bhasma is prepared
comprising the steps:
Cleaning of Shankh
Subjecting cleaned Shankh to Shankh Shodhana resulting in Shodhit Shankh
Incineration of the Shodhit Shankh by Shankh ·Marana resulting in Bhasma Powder.
Converting the Bhasma Powder into finely powdered Shankh Bhasma.
10. The process as claimed in claim 9, wherein small Shankh pieces are cleaned by
washing with hot water.
11. The process as claimed m claims 9 and 10, wherein cleaned Shankh pieces
bundled in muslin cloth are immersed and boiled for up to 3-6 hours into sufficient
amount of lemon juice to obtained Shodhit Shankh.
12. The process as claimed in claim 11, wherein the lemon juice is in an amount of
1:4to 1:16.
13. The process as claimed in claim 12, wherein the lemon juice is preferably in an
amount of 1 :8.
14. The process as claimed in claims 1 0 to 13, wherein the Shodhit Shankh is
incinerated for 4-8 hours at 700-800°C in Muffle Furnace for obtaining Bhasma Powder.
15. The process as claimed in claim 14, wherein the Bhasma Powder is soaked in
water overnight and dried in a oven preferably at a temperature between 50-60°C.
16. The process as claimed in claim 15, wherein the dried Bhasma Powder is passed
through #80 mesh S.S. sieve to obtain finely powdered Shankh Bhasma.
17. The process as claimed in claim 16, wherein the Shankh Bhasma is converted into
natural calcium composition comprising the steps:
1. Soaking the Shankh Bhasma in sufficient amount of fresh lemon juice to
form a soaked bulk.
2. Agitating the soaked bulk of step 1 intermittently.
3. Drying the soaked bulk in an oven at 40-50°C to form dried bulk.
4. Passing the dried bulk of step 3 through #40 mesh S.S. sieve resulting in
the natural calcium composition.
18. The natural calcium composition as claimed in claim 1 is in form of fine powder,
granule, flake or any other suitable form and used as pharmaceutical supplement , food
and beverage additive etc.

Documents

Application Documents

# Name Date
1 138-del-2013-Correspondence Others-(01-02-2013).pdf 2013-02-01
2 138-del-2013-Assignment-(01-02-2013).pdf 2013-02-01
3 138-del-2013-Form-5.pdf 2013-08-20
4 138-del-2013-Form-2.pdf 2013-08-20
5 138-del-2013-Form-1.pdf 2013-08-20
6 138-del-2013-Correspondence-others.pdf 2013-08-20
7 138-del-2013-Correspondence-others (postdate)(16-01-2014).pdf 2014-01-16
8 138-del-2013-Post-Dating-Request-(12-02-2014).pdf 2014-02-12
9 138-del-2013-GPA-(18-03-2014).pdf 2014-03-18
10 138-del-2013-Form-5-(18-03-2014).pdf 2014-03-18
11 138-del-2013-Form-2-(18-03-2014).pdf 2014-03-18
12 138-del-2013-Form-1-(18-03-2014).pdf 2014-03-18
13 138-del-2013-Drawigns-(18-03-2014).pdf 2014-03-18
14 138-del-2013-Description (Complete)-(18-03-2014).pdf 2014-03-18
15 138-del-2013-Correspondence-Others-(18-03-2014).pdf 2014-03-18
16 138-del-2013-Claims-(18-03-2014).pdf 2014-03-18
17 138-del-2013-Abstract-(18-03-2014).pdf 2014-03-18
18 138-del-2013-GPA-(02-04-2014).pdf 2014-04-02
19 138-del-2013-Correspondence-Others-(02-04-2014).pdf 2014-04-02
20 138-del-2013-Description(Provisional).pdf 2014-05-28
21 138-DEL-2013-Form-3-(07-08-2014).pdf 2014-08-07
22 138-DEL-2013-Correspondence-Others-(07-08-2014).pdf 2014-08-07
23 138-del-2013-Correspondence Others-(25-02-2016).pdf 2016-02-25
24 138-DEL-2013-FER.pdf 2018-02-13
25 138-DEL-2013-OTHERS [10-08-2018(online)].pdf 2018-08-10
26 138-DEL-2013-FER_SER_REPLY [10-08-2018(online)].pdf 2018-08-10
27 138-DEL-2013-COMPLETE SPECIFICATION [10-08-2018(online)].pdf 2018-08-10
28 138-DEL-2013-CLAIMS [10-08-2018(online)].pdf 2018-08-10
29 138-DEL-2013-Correspondence to notify the Controller [12-07-2021(online)].pdf 2021-07-12
30 138-DEL-2013-Written submissions and relevant documents [27-07-2021(online)].pdf 2021-07-27
31 138-DEL-2013-US(14)-HearingNotice-(HearingDate-13-07-2021).pdf 2021-10-17
32 138-DEL-2013-US(14)-HearingNotice-(HearingDate-09-02-2024).pdf 2024-01-17
33 138-DEL-2013-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [05-02-2024(online)].pdf 2024-02-05
34 138-DEL-2013-US(14)-ExtendedHearingNotice-(HearingDate-04-03-2024).pdf 2024-02-06
35 138-DEL-2013-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [01-03-2024(online)].pdf 2024-03-01
36 138-DEL-2013-FORM-26 [01-03-2024(online)].pdf 2024-03-01
37 138-DEL-2013-Correspondence to notify the Controller [01-03-2024(online)].pdf 2024-03-01
38 138-DEL-2013-US(14)-ExtendedHearingNotice-(HearingDate-15-03-2024).pdf 2024-03-04
39 138-DEL-2013-Correspondence to notify the Controller [13-03-2024(online)].pdf 2024-03-13
40 138-DEL-2013-Written submissions and relevant documents [29-03-2024(online)].pdf 2024-03-29

Search Strategy

1 138_DEL_20131_13-02-2018.pdf