Volume 9, Issue 4, April – 2024 International Journal of Innovative Science and Research Technology

ISSN No:-2456-2165 https://doi.org/10.38124/ijisrt/IJISRT24APR201

Targeted Drug Delivery through the Synthesis of

Magnetite Nanoparticle by Co-Precipitation
Method and Creating a Silica Coating on it
Vahid Hosseini1; Seyed Masoud Ghoreishi Mokri2; Kadomtseva Alena Viktorovna3
1
Dentistry student at Privolzhsky Research Medical University, Nizhny Novgorod, Russia
2
Department of Medicine at Privolzhsky Research Medical University, Nizhny Novgorod, Russia
3
Associate Professor of the Department of General Chemistry at the Federal State Budgetary
Educational Institution of Higher Education "PIMU" of the Ministry of Health of Russia

Abstract:- Billions of dollars are spent annually in the ligands to the surface due to their tendency to create multiple
world to treat and investigate problems caused by drug covalent bonds. Other characteristics of nanoparticles include
side effects. According to the estimation of health chemical and biological stability, the ability to bind to both
researchers, a huge part of people who take medicine hydrophilic and hydrophobic drugs, and the ability to be
suffer from complications caused by it. In this way, the administered by different routes such as oral, inhalation, and
necessity of using a targeted system in order to deliver injection [1] These nanoparticles have the ability to carry
medicine to the targeted place without damaging healthy substances such as drugs in the form of dissolved, trapped,
tissues is felt more than before. In recent years, targeted encapsulated or attached to the nanoparticle matrix [2].
drug delivery systems based on nanoparticles have
received much attention. In the same direction, in this A group of nanoparticles that have an inorganic origin
research, co-precipitation method was used to prepare and are widely used in drug delivery systems are magnetic
magnetic nanoparticles using iron(|) and iron(||) oxides, iron nanoparticles that are chemically or biologically
and further, according to the synthesis steps of magnetite synthesized. Due to their magnetic properties, these particles
nanoparticles (MNPs) and the mechanism of formation can be directed to a specific place in the body by an external
and identification of magnetite nanoparticles ( Fe₃O₄) by magnetic field, therefore they are very useful and valuable in
examining the infrared pattern (FT-IR) obtained from the field of targeted drug delivery. From this category, we can
Fe₃O₄ nanoparticles, the results of the magnetometric test mention magnetite and maghemite nanoparticles, which have
(VSM) of Fe₃O₄ nanoparticles, X-ray diffraction pattern received a lot of attention in drug delivery. One of the most
(XRD) of Fe₃O₄ nanoparticles, Field Emission Scanning important advantages of magnetic nanoparticles is that they
Electron Microscope (FE-SEM) images obtained from can be easily modified [3].
Fe₃O₄ nanoparticles was discussed. After this stage, silica-
coated iron nanoparticles (Fe₃O₄@SiO₂) were prepared, In recent years, many methods have been designed and
and the infrared (FT-IR) pattern of Fe₃O₄@SiO₂) was also introduced for the production of magnetic nanoparticles, and
investigated. It is worth mentioning that the mechanism in most of them, the focus is on obtaining a controlled shape,
of formation and identification of magnetic silica-coated high stability and size of nanoparticles. The method used for
iron nanoparticles (Fe₃O₄@SiO₂) has been described in the synthesis of magnetic nanoparticles depends on the type
detail. Therefore, the obtained results indicate that the of properties of the desired material, which can be chosen
drug can be guided in a controlled and targeted manner after determining the properties of the desired product
by the magnetic field, and the results of the FE-SEM according to the shape, distribution and economic aspects.
images show that the obtained product has a spherical Among the methods that have been designed so far, we can
morphology and the particle size distribution was less mention the sol-gel method 5, co-precipitation, hydrothermal,
than 100 nm. Therefore, spherical shape and the combustion, sonochemical and microemulsion methods [4-
symmetry of these particles can be helpful for their 5].
movement in the liquid mediu.
II. CO-PRECIPITATION METHOD TO PREPARE
MAGNETIC NANOPARTICLES
Keywords:- Targeted Drug Delivery - Magnetite
Nanoparticle - Co-Precipitation Method - Silica Coating It is one of the oldest methods of synthesis of magnetic
nanoparticles, which was used for the first time to produce
I. INTRODUCTION magnetite nanoparticles. Among the advantages of this
method, it can be mentioned that it is a single step, easy, cost-
In general definition, it can be said that the particles of effective and fast, which produces a small and uniform
sizes in the range of (10-100) nanometers are called product. In this method, iron(Ⅱ) and iron(Ⅲ) oxides and a
nanoparticles. Nanoparticles, due to their very small size and base are used and magnetite nanoparticles can be synthesized.
high surface-to-volume ratio, can be used to attach multiple Among the effective parameters in the production of these

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Volume 9, Issue 4, April – 2024 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165 https://doi.org/10.38124/ijisrt/IJISRT24APR201

nanoparticles, we can mention the ionic strength, the type of (Ⅲ) ions, which are effective in the size, shape and
salt used, the reaction temperature, pH, the speed of stirring composition of the synthesized nanoparticles [6].
the reaction and adding base, and the ratio of iron (Ⅱ) and iron

 Steps of of Magnetite Nanoparticles (MNPs) Synthesis:

Co-precipitation method was used for the synthesis of III. MECHANISM OF FORMATION AND
nanoparticles in this research [7]. For this purpose, 4.5 grams IDENTIFICATION OF MAGNETITE
of FeCl₃.6H₂O and 2 grams of FeCl₂.4H₂O in 100 ml of NANOPARTICLES (FE₃O₄)
double-distilled water were added to a fume hood equipped
with nitrogen inlet and outlet, The resulting mixture was To prepare these nanoparticles, a co-precipitation
vigorously stirred with a magnetic stirrer under reflux method was used, in which iron (Ⅱ) and iron (Ⅲ) salts were
conditions and a temperature of 85°C for 15 minutes, then 15 used with stoichiometric ratios of 1 to 2 according to the
ml of 30% ammonia solution was added drop by drop to the following reaction:
mixture, the color of the mixture immediately changed from
orange to black. The resulting solution was refluxed for 30 By adding ammonia to the reaction solution containing
minutes. After the reaction is over, the precipitate was iron salts, spherical shape and black iron nanoparticles are
separated by a magnet and washed 3 times with double- obtained as follows.
distilled water. The black precipitate of Fe₃O₄ obtained from
this step was identified by FT-IR, VSM and SEM analyses

Fig 1: Magnetite preparation reaction

Fig 2: General Scheme of Preparation of Magnetite Nanoparticles

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Volume 9, Issue 4, April – 2024 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165 https://doi.org/10.38124/ijisrt/IJISRT24APR201

Magnetic iron nanoparticles are oxidized in air and prevent oxidation, nanoparticles were synthesized in the
produce Fe(OH)₃ according to the reaction shown below. To presence of nitrogen gas.

 Examining the infrared pattern (FT-IR) of Fe₃O₄ increase of H, the amount of M increases until it reaches its
nanoparticles: highest level, which is called the saturation magnetization
Diagram 1- shows the FT-IR spectrum of the prepared (Ms). The resulting diagram shows a residual magnetic value
Fe₃O₄ compound. The two bands appearing at 430 Cm⁻¹and after removing the external field, which is called
560 Cm⁻¹correspond to the vibrations of the Fe—O bonds of "hysteresis loop ". The presence of this loop indicates that
the compound [8]. The band related to surface OH groups can after the removal of the external magnetic field, some
also be seen in the range of Cm⁻¹3400. magnetic property remains in the material and all the
magnetic property of the ferromagnetic material is not lost.
Because after the removal of the external magnetic field, the
orientation of the atomic magnetic moments in all areas do
not return to their original arrangement. Therefore, even when
the value of the external field H reaches zero, there is still
some residual magnetization MR in the material, which can
only be removed by applying a coercive HC field, opposite to
the initial field direction. In the magnetization diagram of
single-domain magnetic materials, no hysteresis loop is
observed, such compounds are called super-paramagnetic.
Magnetite nano-oxides smaller than 100 nm have
superparamagnetic properties at room temperature. [9]

Diagram 1: FT-IR Spectrum of Magnetite Nanoparticles

 Examining the Results of the Magnetometery Test (VSM)

of Fe₃O₄ Nanoparticles:
In paramagnetic materials, the arrangement of atomic
magnetic moments is completely random and separate, so that
the magnetic moment of the entire crystal structure is zero. In
this case, if these materials are exposed to an external
magnetic field, some of these separate atomic magnetic
moments will find the same orientation and the structure will Fig 3: Changes of Magnetic Susceptibility in a
have a small amount of magnetic moment. In the Ferromagnetic Material
ferromagnetic state, the atomic magnetic moments have the
same orientation relative to each other. Therefore, the crystal Diagram 2- shows the magnetic behavior of magnetite
structure has a total magnetic moment. This is despite the fact nanoparticles, which was investigated by performing
that in an antiferromagnetic crystal, half of the atomic vibrational magnetometer analysis of the VSM sample. As
magnetic moments are directed upwards and the other half are can be seen, the obtained magnetite particles show the
directed downwards. Therefore, the total magnetic moment characteristic of super para magnetism with a maximum
for an antiferromagnetic crystal is zero. Figure 2 shows the magnetic susceptibility of 70 emu/g. The absence of a
magnetic susceptibility diagram of a ferromagnetic material hysteresis loop in the magnetic susceptibility diagram is a
with magnetic strength M in the presence of an external confirmation of the superparamagnetic behavior of magnetite
magnetic field with strength H. As it can be seen, with the in the presence of an external magnetic field.

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Volume 9, Issue 4, April – 2024 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165 https://doi.org/10.38124/ijisrt/IJISRT24APR201

Diagram 2: Magnetometric Diagram of Magnetite Nanoparticles

 Examining the X-Ray Diffraction (XRD) Pattern of Fe₃O₄

Nanoparticles
The X-ray diffraction pattern of Fe₃O₄ compound is
shown in Figure 3. Comparing this pattern with the reference
magnetite pattern in the aforementioned device with JCPDS
No. 0629-19, which belongs to Fe₃O₄, determined that all the
diffraction signals related to the prepared magnetite structure
are consistent with the diffraction related to the reference
magnetite structure in terms of the position and intensity of
vibrations, which is a confirmation of the formation of the
Fe₃O₄ compound.

Fig 4: FESEM Images Obtained from Magnetite

Nanoparticles

 Preparation of Silica Coated Iron Nanoparticles

(Fe₃O₄@SiO₂)
Silica coated iron nanoparticles were prepared with a
slight change according to the method of Liu et al. [10] In this
step, 3 grams of Fe₃O₄ nanoparticles obtained from the
previous step were transferred to a double-mouth flask and 80
ml of tetra ethyl ortho silicate (TEOS) solution 10% by
volume in deionized water was added to it. Then, 60 ml of
glycerol was added to the mixture and the pH of the resulting
suspension was adjusted by acetic acid to about 4.5. At the
Diagram 3: X-ray Diffraction Pattern of end, the resulting mixture was stirred under reflux at a
Magnetite Nanoparticles temperature of 90°C for 2 hours with a magnetic stirrer. At
the end, the resulting contents were transferred to a beaker,
 Examining the Scanning Electron Microscope (FE-SEM) the sediment was separated by a magnet, and washed with
Images Obtained from Fe₃O₄ Nanoparticles double-distilled water and methanol, respectively. After
Scanning electron microscope is used to determine drying at room temperature, the resulting nanoparticles were
surface morphology, texture, size and shape of major samples identified by FT-IR spectroscopy.
of solid materials. The FE-SEM images obtained from the
Fe₃O₄ compound in this project are shown in Figure 3. As can  Mechanism of Formation and Identification of Silica
be seen, the obtained nanoparticles are assemblies of Coated Magnetic Iron Nanoparticles (Fe₃O₄@SiO₂)
spherical particles stuck together with a high surface area and In order to prevent magnetite nanoparticles from
an approximate size of 20-30 nm. oxidizing, an inert layer of silica is placed between the iron
core and the reaction medium. It is possible to perform this
operation with the sol-gel technique and by adding the TEOS
compound to the solution containing magnetite nanoparticles
[11].

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Volume 9, Issue 4, April – 2024 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165 https://doi.org/10.38124/ijisrt/IJISRT24APR201

Among the effects of silicon coating on magnetite vibrations of the Si—O—Si bond, which appeared in the
nanoparticles, we can mention protecting them against range of Cm⁻¹980 and Cm⁻¹1080, respectively. [13] The
oxidation, creating a suitable space for modifying the surface broad band appearing in the range of Cm⁻¹3400 indicates the
of nanoparticles, and also increasing their thermal stability. presence of OH bonds on the surface of these nanoparticles
Another important advantage of this process is the increase in [14].
the number of hydroxyl groups on the surface of
nanoparticles, which causes better functionalization on the
surface of nanoparticles. Also, the silica coating prevents the
clumping of nanoparticles and the distribution of particles in
the solution environment is better [12].

The mechanism of this process is shown below in Figure

4. First, TEOS molecules are formed in the vicinity of glacial
acetic acid and glycerol hydrolysis, followed by hydroxyl
groups. Adding glycerol to the solution causes the
nanoparticles to be completely separated and the silica
coating is done more effectively. The reason for adding acid
is to adjust the pH of the solution in order to hydrolyze the
OH groups on the surface of nanoparticles and TEOS Diagram 4: FT-IR Spectrum of Magnetite Nanoparticles
molecules, and as a result, these molecules are effectively Coated with Silica
connected to each other. A scheme of silica coating process
on magnetite nanoparticles is shown in Figure 5: IV. CONCLUSIONS

In this research, an attempt has been made to provide a

method in which the medicine can be controlled and directed
by the magnetic field. The results of examining the FE-SEM
images show that the obtained product had a spherical
morphology and the particle size distribution was less than
100 nm. The spherical and symmetrical shape of these
particles can help them move in the liquid environment.
Analysis of the thermal decomposition of the final product
also indicates the presence of both organic and mineral
substances in the drug part and the magnetic part of the
Fig 5: Hydrolysis Mechanism of TEOS Molecules
sample.

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