U.S. patent application number 17/020107 was filed with the patent office on 2020-12-31 for calcium hydroxide nanoparticles synthesized with carob pulp extract.
The applicant listed for this patent is KING SAUD UNIVERSITY. Invention is credited to OSAMA GHURMULLAH M. ALGHAMDI, RAWAN IBRAHIM SALEM ALKHALAF, MOHAMMED GHAZI ALKINDI, HAJERSAAD ABDULLAH ALLAYED, NASSER RAQE RASHED ALQHTANI, MOHAMAD SALEH ALSALHI, SANDHANSAMY DEVANESAN.
Application Number | 20200405749 17/020107 |
Document ID | / |
Family ID | 1000005086870 |
Filed Date | 2020-12-31 |
United States Patent
Application |
20200405749 |
Kind Code |
A1 |
ALSALHI; MOHAMAD SALEH ; et
al. |
December 31, 2020 |
CALCIUM HYDROXIDE NANOPARTICLES SYNTHESIZED WITH CAROB PULP
EXTRACT
Abstract
Calcium hydroxide nanoparticles (Ca(OH).sub.2NPs) synthesized
using carob pulp extract may be hexagonal nanoparticles with a
diameter ranging from about 31.22 nm to about 81.22 nm. The
Ca(OH).sub.2NPs may be synthesized by heating ethylene glycol,
adding calcium hydroxide to the ethylene glycol to provide a first
mixture, heating the first mixture, adding a carob pulp aqueous
extract to the first mixture to form a second mixture, heating the
second mixture, adding sodium hydroxide (NaOH) to the second
mixture to form a third mixture, heating the third mixture, resting
the third mixture at room temperature after heating, centrifuging
the third mixture, collecting a colloid sediment, extracting any
unwanted contaminants from the colloid sediment, and drying the
colloid sediment to obtain Ca(OH).sub.2NPs.
Inventors: |
ALSALHI; MOHAMAD SALEH;
(Riyadh, SA) ; DEVANESAN; SANDHANSAMY; (Riyadh,
SA) ; ALKHALAF; RAWAN IBRAHIM SALEM; (Qassim, SA)
; ALLAYED; HAJERSAAD ABDULLAH; (Riyadh, SA) ;
ALQHTANI; NASSER RAQE RASHED; (Riyadh, SA) ; ALKINDI;
MOHAMMED GHAZI; (Riyadh, SA) ; ALGHAMDI; OSAMA
GHURMULLAH M.; (Riyadh, SA) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
KING SAUD UNIVERSITY |
Riyadh |
|
SA |
|
|
Family ID: |
1000005086870 |
Appl. No.: |
17/020107 |
Filed: |
September 14, 2020 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
16397286 |
Apr 29, 2019 |
10780111 |
|
|
17020107 |
|
|
|
|
Current U.S.
Class: |
1/1 |
Current CPC
Class: |
A61K 9/1682 20130101;
C01P 2002/85 20130101; A61K 9/1652 20130101; C01P 2002/76 20130101;
C01F 11/02 20130101; C01P 2004/03 20130101; B01D 11/0288 20130101;
C01P 2002/01 20130101; C01P 2004/64 20130101; A61K 33/08 20130101;
C01P 2002/72 20130101; C01P 2002/82 20130101 |
International
Class: |
A61K 33/08 20060101
A61K033/08; C01F 11/02 20060101 C01F011/02; B01D 11/02 20060101
B01D011/02; A61K 9/16 20060101 A61K009/16 |
Claims
1-20. (canceled)
21. A method of treating dental diseases, comprising: providing
calcium hydroxide nanoparticles, wherein the calcium hydroxide
nanoparticles are synthesized by: (a) heating ethylene glycol,
wherein heating the ethylene glycol is performed in an ultrasonic
water bath heated to a temperature of about 99.9.degree. C.; (b)
adding calcium hydroxide to the ethylene glycol to form a first
mixture; (c) heating the first mixture, wherein heating the first
mixture is performed in an ultrasonic water bath heated to a
temperature of about 99.9.degree. C.; (d) adding a carob pulp
aqueous extract to the first mixture to form a second mixture; (e)
heating the second mixture wherein heating the second mixture is
performed in an ultrasonic water bath heated to a temperature of
about 99.9.degree. C.; (f) adding sodium hydroxide to the second
mixture to form a third mixture; (g) heating the third mixture
wherein heating the third mixture is performed in an ultrasonic
water bath heated to a temperature of about 99.9.degree. C.; (h)
resting the third mixture after heating; (i) centrifuging the third
mixture and collecting a colloid sediment, wherein the centrifuging
is at 1500 rpm for 30 minutes and repeated a plurality of times;
(j) extracting chemical contaminants from the colloid sediment to
provide a purified colloid sediment; and (k) drying the purified
colloid sediment to obtain the Ca(OH).sub.2 nanoparticles, wherein
the nanoparticles have a minimum diameter of 31.22 nm and a maximum
diameter of 81.22 nm; formulating a pharmaceutical composition by
adding a pharmaceutically acceptable carrier; and administering the
pharmaceutical composition to a patient in need thereof.
22. The pharmaceutical composition of claim 21, wherein the dental
disease is a dental abscess.
23. The pharmaceutical composition of claim 21, wherein the
pharmaceutical composition is compounded in a unit dosage form, the
unit dosage form selected from the group consisting of tablets,
pills, capsules, powders, granules, ointments, sterile parenteral
solutions, sterile suspensions, metered aerosol sprays, metered
liquid sprays, drops, ampules, auto-injector devices, and
suppositories.
Description
CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application is a division of Ser. No. 16/397,286, filed
Apr. 29, 2019, now pending.
BACKGROUND
1. Field
[0002] The disclosure of the present patent application relates to
nanotechnology, and particularly to a method of synthesizing
calcium hydroxide nanoparticles using carob pulp extract.
2. Description of the Related Art
[0003] In materials science, nanomaterials have demonstrated unique
size and morphology based characteristics. Nanotechnology is an
emerging field demonstrating significant potential for the
development of new medicines. The most common methods of producing
nanoparticles are chemical or mechanical, including ball milling,
thermal quenching, precipitation techniques, and vapor deposition.
However, these methods are often costly, and may result in toxic
byproducts.
[0004] Biological approaches for synthesizing nanoparticles can
avoid many of the disadvantages associated with the chemical or
mechanical synthesis methods.
[0005] Thus, calcium hydroxide nanoparticles synthesized with carob
pulp extract solving the aforementioned problems are desired.
SUMMARY
[0006] Calcium hydroxide nanoparticles (Ca(OH).sub.2NPs)
synthesized using carob pulp extract may be hexagonal nanoparticles
with a diameter ranging from about 31.22 nm to about 81.22 nm. The
Ca(OH).sub.2NPs may be synthesized by heating ethylene glycol,
adding calcium hydroxide to the ethylene glycol to provide a first
mixture, heating the first mixture, adding a carob pulp aqueous
extract to the first mixture to form a second mixture, heating the
second mixture, adding sodium hydroxide (NaOH) to the second
mixture to form a third mixture, heating the third mixture, resting
the third mixture at room temperature after heating, centrifuging
the third mixture, collecting a colloid sediment, extracting any
unwanted contaminants from the colloid sediment, and drying the
colloid sediment to obtain Ca(OH).sub.2NPs. The Ca(OH).sub.2NPs may
be useful in a wide variety of applications including but not
limited to water purification, paper preservation, antimicrobial
agent applications, and in treating dental diseases, including but
not limited to dental abscesses.
[0007] An embodiment of the present subject matter is directed to a
composition including Ca(OH).sub.2NPs and carob pulp extract.
[0008] An embodiment of the present subject matter is directed to a
pharmaceutical composition comprising the Ca(OH).sub.2NPs and a
pharmaceutically acceptable carrier.
[0009] An embodiment of the present subject matter is directed to a
method of making a pharmaceutical composition including mixing the
Ca(OH).sub.2NPs with a pharmaceutically acceptable carrier.
[0010] These and other features of the present disclosure will
become readily apparent upon further review of the following
specification and drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] FIG. 1 depicts an X-ray diffraction spectrum of the calcium
hydroxide nanoparticles synthesized with carob pulp extract.
[0012] FIG. 2 depicts an attenuated total reflectance
Fourier-transform infrared spectrum of the calcium hydroxide
nanoparticles synthesized with carob pulp extract.
[0013] FIG. 3 depicts a transmission electron micrograph of the
calcium hydroxide nanoparticles synthesized with carob pulp
extract.
[0014] FIG. 4 depicts a scanning electron micrograph of the calcium
hydroxide nanoparticles synthesized with carob pulp extract.
[0015] FIG. 5 depicts an energy dispersive X-ray spectrum of the
calcium hydroxide nanoparticles synthesized with carob pulp
extract.
[0016] Similar reference characters denote corresponding features
consistently throughout the attached drawings.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] Calcium hydroxide nanoparticles synthesized using carob pulp
extract may be hexagonal nanoparticles with a diameter ranging from
about 31.22 nm to about 81.22 nm. The Ca(OH).sub.2NPs may be
synthesized by heating ethylene glycol, adding calcium hydroxide to
the ethylene glycol to provide a first mixture, heating the first
mixture, adding a carob pulp aqueous extract to the first mixture
to form a second mixture, heating the second mixture, adding sodium
hydroxide (NaOH) to the second mixture to form a third mixture,
heating the third mixture briefly, resting the third mixture after
heating, centrifuging the third mixture at least once, collecting a
colloid sediment, extracting any unwanted contaminants from the
colloid sediment, and drying the colloid sediment to obtain
Ca(OH).sub.2NPs. In an embodiment, unwanted contaminants can be
extracted in isopropanol. The Ca(OH).sub.2NPs may be useful in a
wide variety of applications, including but not limited to, water
purification, paper preservation, antimicrobial applications, and
in treating dental diseases, including but not limited to dental
abscesses.
[0018] In an embodiment, the heating may be performed in an
ultrasonic water bath heated to a temperature of about 99.9.degree.
C. In an embodiment, the ethylene glycol is heated in an ultrasonic
water bath for about 10 minutes at about 99.9.degree. C. In an
embodiment, the first mixture is heated in an ultrasonic water bath
for about 15 minutes at about 99.9.degree. C. In an embodiment, the
second mixture is heated in an ultrasonic water bath for about 15
minutes at about 99.9.degree. C. In an embodiment, the third
mixture is heated in an ultrasonic water bath for about 5 minutes
at about 99.9.degree. C.
[0019] As used herein, the term "about," when used to modify a
numerical value, means within ten percent of that numerical
value.
[0020] In an embodiment, the carob pulp aqueous extract may be
synthesized by collecting carob fruit, drying the carob fruit to
provide a dried carob fruit, and reducing the dried carob fruit to
a fine powder. For example, the dried carob fruit, e.g., pulp
and/or seeds, can be ground to produce the carob fruit powder. The
carob fruit powder can be suspended in a liquid, e.g., water. The
suspension can be filtered to produce the carob pulp aqueous
extract. In an embodiment, the suspension can be filtered using
Whatman.RTM. No. 1 filter paper to produce the carob pulp aqueous
extract.
[0021] In an embodiment, the carob fruit used to synthesize the
carob pulp aqueous extract may be grown in Saudi Arabia. In an
embodiment, 1 Kg of carob fruit may be used to make the carob pulp
aqueous extract.
[0022] In an embodiment, about 50 ml of ethylene glycol is heated
in the ultrasonic water bath for about 10 minutes. Then, about 25 g
of calcium hydroxide is added to the ethylene glycol to form the
first mixture. The calcium hydroxide and ethylene glycol solution
may be stirred in the ultrasonic water bath until the calcium
hydroxide is completely dissolved (about 15 minutes). About 50 ml
of carob pulp aqueous extract is slowly added to the first mixture
in the ultrasonic water bath over a period of about 15 minutes to
form the second mixture. A 1 M concentration of NaOH is then slowly
added to the second mixture in the ultrasonic water bath over a
period of about 5 minutes to form the third mixture. The third
mixture is rested at room temperature.
[0023] In an embodiment the third mixture is centrifuged at about
15000 RPM for about 30 minutes. The supernatant is then discarded
and a colloid sediment is collected. Unwanted contaminants from the
colloid sediment can be removed from the colloid sediment by mixing
isopropanol with the colloid sediment and centrifuging the mixture
of isopropanol and colloid sediment at about 15000 RPM for about 30
minutes. The process of extracting unwanted chemical contaminants
from a colloid sediment obtained from a centrifugation cycle (by
mixing isopropanol with the colloid sediment and centrifuging the
mixture of isopropanol and colloid sediment) can be repeated one or
more times, e.g., three or four times, to extract unwanted chemical
contaminants from the colloid sediment
[0024] An embodiment of the present subject matter is directed to a
composition including Ca(OH).sub.2NPs and carob pulp extract.
[0025] An embodiment of the present subject matter is directed to a
pharmaceutical composition comprising the Ca(OH).sub.2NPs and a
pharmaceutically acceptable carrier.
[0026] An embodiment of the present subject matter is directed to a
method of making a pharmaceutical composition including mixing the
Ca(OH).sub.2NPs with a pharmaceutically acceptable carrier. For
example, the method of making a pharmaceutical composition can
include mixing the Ca(OH).sub.2NPs under sterile conditions with a
pharmaceutically acceptable carrier with preservatives, buffers,
and/or propellants to create the pharmaceutical composition.
[0027] An embodiment of the present subject matter is directed to a
pharmaceutical composition including the Ca(OH).sub.2NPs. To
prepare the pharmaceutical composition, the Ca(OH).sub.2NPs, as the
active ingredient, are intimately admixed with a pharmaceutically
acceptable carrier according to conventional pharmaceutical
compounding techniques. Carriers are inert pharmaceutical
excipients, including, but not limited to, binders, suspending
agents, lubricants, flavorings, sweeteners, preservatives, dyes,
and coatings. In preparing compositions in oral dosage form, any of
the pharmaceutical carriers known in the art may be employed. For
example, for liquid oral preparations, suitable carriers and
additives include water, glycols, oils, alcohols, flavoring agents,
preservatives, coloring agents, and the like. Further, for solid
oral preparations, suitable carriers and additives include
starches, sugars, diluents, granulating agents, lubricants,
binders, disintegrating agents, and the like.
[0028] The present compositions can be in unit dosage forms, such
as tablets, pills, capsules, powders, granules, ointments, sterile
parenteral solutions or suspensions, metered aerosol or liquid
sprays, drops, ampules, auto-injector devices or suppositories, for
oral parenteral, intranasal, sublingual or rectal administration,
or for administration by inhalation or insufflation. The active
compound can be mixed under sterile conditions with a
pharmaceutically acceptable carrier and, if required, any needed
preservatives, buffers, or propellants. The composition can be
presented in a form suitable for daily, weekly, or monthly
administration. The pharmaceutical compositions herein will
contain, per dosage unit, e.g., tablet, capsule, powder, injection,
teaspoonful, suppository and the like, an amount of the active
ingredient necessary to deliver an effective dose.
[0029] The following examples illustrate the present teachings.
Example 1
Synthesis of Calcium Hydroxide Nanoparticles with Carb Pulp
Extract
[0030] Carob pulp aqueous extract was produced by washing carob
fruits with tap water and deionized water, drying the fruit under
laboratory conditions, grinding the dried fruit to a fine powder,
soaking the powder in water, and filtering extract with Whatman No.
1 filter paper. Calcium hydroxide nanoparticles were synthesized
with the Carob pulp extract as follows. Ethylene glycol (about 50
ml) was placed in a conical flask in an ultrasonic water bath for
ten minutes at the maximum temperature of 99.9.degree. C. About 25
g of calcium hydroxide was added to the ethylene glycol solution
under constant stirring until the calcium hydroxide completely
dissolved (about 15 minutes). The resulting first mixture appeared
as a thick suspension. The Carob pulp aqueous extract (about 50 ml)
was slowly added to the first mixture under constant stirring at a
maximum temperature of 99.9.degree. C. over a period of about 15
minutes, producing a second mixture. Sodium hydroxide (1 M) was
then slowly added to the second mixture at the maximum temperature
of 99.9.degree. C. over about 5 minutes, and the resulting third
mixture was allowed to rest without stirring. The third mixture was
then centrifuged at 15,000 RPM for about 30 minutes, the
supernatant was discarded, and the colloid sediment was collected.
A volume of isopropanol was added to the colloid sediment, mixed
well and centrifuged at 15,000 RPM for about 15 minutes. The
supernatant was discarded and the colloid sediment was collected.
The process of collecting the colloid sediment after centrifuging,
mixing the colloid sediment with isopropanol, and centrifuging the
resulting mixture was repeated three times. The final resulting
colloid sediment was then dried to form a Ca(OH).sub.2NP
powder.
Example 2
Confirmation of Calcium Hydroxide Nanoparticles Synthesis with Carb
Pulp Extract
[0031] Ca(OH).sub.2NPs produced according to the method of Example
1 were analyzed as follows.
[0032] X-ray diffraction of the Ca(OH).sub.2NPs revealed four
distinct peaks at 30.90, 32.06, 60.52, and 70.08 2 .theta. degrees,
respectively (FIG. 1). These peaks confirm the presence of calcium
hydroxide nanoparticles at a high degree of purity.
[0033] The attenuated total reflection (ATR) spectrum of the
Ca(OH).sub.2NPs confirmed the presence of functional groups, such
as carbonyls, alcohols, carboxylic acids, esters, and amines in the
Ca(OH).sub.2NPs (FIG. 2). The spectrum shows three bands, including
one at 1041.36 cm.sup.-1 corresponding to a C--OH(OH) group, a
stretching vibration band at 1341.49 cm.sup.-1 corresponding to a
C--C group, and a band at 1600.49 cm.sup.-1 corresponding to a
CO--NH group. These results confirm organic mediated synthesis of
Ca(OH).sub.2NPs.
[0034] Transmission electron microscopy (TEM) was used to
characterize the size and shape of the Ca(OH).sub.2NPs. The
Ca(OH).sub.2NPs were found to be hexagonal, with a minimum diameter
of about 31.22 nm and a maximum diameter of about 81.22 nm (FIG.
3).
[0035] Scanning electron microscopy was used to confirm the
structural findings of TEM. Scanning electron micrographs of the
Ca(OH).sub.2NPs confirmed that the nanoparticles have hexagonal
shapes and sizes in the nano range (FIG. 4).
[0036] Energy dispersive X-ray analysis (EDS) was used to determine
the inorganic and organic components of the Ca(OH).sub.2NPs. The
EDS spectrum demonstrates that the Ca(OH).sub.2NPs have oxygen,
nitrogen, zinc, magnesium, and calcium (FIG. 5).
[0037] It is to be understood that the calcium hydroxide
nanoparticles synthesized with carob pulp extract are not limited
to the specific embodiments described above, but encompass any and
all embodiments within the scope of the generic language of the
following claims enabled by the embodiments described herein, or
otherwise shown in the drawings or described above in terms
sufficient to enable one of ordinary skill in the art to make and
use the claimed subject matter.
* * * * *