To Load Ibuprofen Drug Into Prepared Silica Biology

Table of Content

The chief purpose of the undertaking is to Load Ibuprofen drug in to prepared silicon oxide and to detect the drug release in a individual measure procedure. Silica was prepared with Sodium dodecyl sulfate, which is anionic wetting agent ( SDS ) and Tween20, which is Polysorbate wetting agent and with Ammonia.

Ibuprofen Sodium ( IBU-Na ) is used as drug to lade in silicon oxide. By lading this drug in to prepared silicon oxide and successfully laden drug in to silica. Then found the Invitro drug release.

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Sodium dodecyl sulfate prepared silica dug is loaded successfully and surface country is measured. Surface country found as less than 1, but optical density of the drug release was good. Tween20 prepared silica drug is loaded successfully as in SDS and the surface country in tween20 less than 1, but drug release was good.

Ammonia samples, Prepared in 3 batches like B1, B2, B3. For each batch drug loaded successfully and surface country is measured. Silica prepared with ammonium hydroxide shows better surface country than SDS and Tween20. This sample shows 26.1 m2/gm and the drug release is besides shows good public presentation with ammonium hydroxide because the drug holding Na salt and ammonium hydroxide holding alkalic belongingss. By comparing all’t ‘ values these Ammonia samples shows speedy release of drug.

Silicon is the 1 of the burgeoning mineral in the Earth crust. Silica is largely utile in the human activities now yearss. In general silicon oxide is found in several natural ways like in clay, glass and chemically derived the merchandises like silicon oxide, ceramics. Silica and silicates are besides available in the signifier of an formless white pulverization which is made synthetically, by two methods 1 ) pyrogenic procedure and 2 ) moisture procedure which is done by precipitated silicon oxide or gels. This formless silicon oxide from the ancient clip it is used in the nutrient merchandises, personal attention merchandises, works protection.4

Siliceous minerals found in different types of construction. Silica and combined minerals are structurally holding tetrahedral agreement of four O atoms surrounded by silicon cardinal atom ( SiO4 ) . The mean each O is distributed by Si ‘s in two tetrahedral in the SiO2 stoichiometry of silicon oxide. Sharing of the silicon oxide edges is terminated and sharing faces do n’t happen by hapless stableness. Some corners remain undistributed by the possibility of associating tetrahedrons. Each undistributed O atom gives a negative charge to the anionic group. 4

It is the celebrated technique to bring forth silicon oxide. It is an easy procedure by the uninterrupted fire hydrolysis of Si tetrachloride, SiCl4. Then SiCl4 alterations into gas after that SiCl4reacted with H and O. Water acts as an intermediate and it reacts with SiCl4 to organize Si.

After this exothermal chemical reaction it generates heavy heat necessitating chilling of the reaction merchandises. Hydrochloric acid, is the by merchandise which is separated from silica pulverization and is separated and recycled and the removed pulverization is used for industry of Si tetrachloride

These concentrations of the reactants show some fluctuations and command the physical and chemical belongingss such as atom size distribution and construction, surface country of the thermic silicon oxide. The usage of silanes makes the accommodation to do the concluding merchandise.

( II ) Precipitated Silica:

In this method of readying we use alkali silicate, Na silicate and acid. It is prepare in different stairss. First, sulfuric acid is taken in to a vas incorporating H2O and stirred smartly. In different instances existed pH is set. Then this all constituents are feeding in to the reactor like this procedure it done in same clip intervals. Normally silicon oxide is manufactured at the pH values greater than 7, and silicon oxide gels are manufactured at pH less than 7.

Na20 X 3.3 SiO2 + H2SO4 3.3 SiO2 + Na2SO4 + H2O ( 4 )

The obtained precipitation obtained is a suspension. The obtained filter bar is washed with Na sulfate and so it is resuspended and allowed for spray prohibitionist. Harmonizing to the drying engineering and the practical size of the silicon oxide it is decently milled and made in to ticket atoms which obey the atom size of the silicon oxide. Even precipitated silicon oxide converted into hydrophilic to hydrophobic by handling with chemicals.

( III ) Silica gels:

This method of readying we use alkali silicate, Na silicate and acid. Silica gels are prepared by the precipitation method. The readying of silicon oxide gels is reacted in little vass. Raw stuffs which are used are taken into sociables in short clip and assorted to organize silicon oxide hydrosols. The pH of the formed hydrosols is less than 7. The given silicon oxide is chiefly dependent on the pH. If the pH of the formation increases the silicon oxide gel formed will be lower. Silica gel follows the aging engineering to modify the gels. In this procedure the silicon oxide gels formed in to some balls make certain the balls are crushed and enter in to farther procedure. By completing this aging silicon oxide should be washed to take the soluble salts. Make the obtained silicon oxide good dried and it should be free from surface H2O. In the drying procedure there should be a opportunity of fall ining the atom size distribution and porousness so to keep a coveted atom size distribution milling should be done. 4

Use of silicon oxide:

Silica is used in the formation of bone. Silica is found to be present unambiguously in the countries of the active growing occurs grow smaller in relationship to the puting down of hydroxyapatite, or bone crystal, by the procedure that transforms fictile bone into a difficult construction. With this silicon oxide acted as a regulation factor for the sedimentation of bone. Silica is besides utile in the tissue upset. 5

Characterization methods of silicon oxide:

Silica is characterized in different methods such as

1.2.1 ) Volume of the pore and pore size distribution:

Pore volume and specific rating methods are non explained clearly. Normally silica ‘s pore volume is known to be ( a ) surface raggedness, ( B ) the nothingness volume ( C ) The sums or atoms ciphering micro or sub microscope volume. Pore volume can be determined by quicksilver porosimetry and the BJH method. By the mensural force per unit area P, a measure of force required to make full quicksilver in to the pores of the silica sample. Then the needed force per unit area is reciprocally relative to the diameter of the pore. At the given force per unit area the volume of quicksilver known so the pore volume can be calculated.

Specific surface of silicon oxide:

This specific surface of silicon oxide can be determined by Brunauer-Emmett-Teller ( BET ) surface assimilation method. The procedure is to chill the silicon oxide sample to the temperature of liquid N because in the low temperatures ‘ N is adsorbed on silica surface. To happen the perfect surface country BET method outputs absolutely. So that it is non merely easy to happen the surface of the sample with N covered sample but besides pores are filled. Then the distribution of the pores can be determined utilizing Barrett-Joyner-Halendar method ( BJH ) .

Cetyltrimethylammonium bromide surface country ( CTAB ) :

The CTAB method comes from C black engineering, and now utilizing in silica engineering. The CTAB method is worked up on the rule of surface assimilation of active molecules from aqueous solutions. The surface assimilation of the CTAB molecules is the outer, geometrical surface.

DBP figure, oil Absorption:

It is involved by the soaking up of Dibutylphtalate ( DBP ) . This all right technique provides an indicant of the full volume of the liquid that can be absorbed by the sample. Due to toxicity of DBP oil, paraffin oil is being replaced.

Microscopic methods:

To happen the dimensions of the silicon oxide there is a alone method which is electron microscopy. This provides the primary atom size, aggregates with certain restrictions on the atom size distribution. Electron microscopic surfaces are calculated from atom size distributions, and these are to be measured with BET methods. There are several types in negatron microscopy

Transmission Electron Microscopy ( TEM ) :

Electrons are allowed to go through from a thin object and those negatrons are holding an interaction with prepared sample, which is used to bring forth an image. The declaration is 1000 which is more than that of light microscopy. The declaration of TEM is 0.2-0.3 nanometers ( nanometer ) and for light microscope is ~200 nm. TEM images will supply valuable information of structural composing in different silicon oxide samples because it is holding high declaration. By this transmittal electron microscopy it is possible to happen the construction of silicon oxide.

Scaning Electron Microscopy ( SEM ) :

It is non a microscopic technique that means it uses electromagnetic lenses for amplifying images. It produces a strongly magnified image with the aid of negatrons. These crisp negatrons produce really good declarations and focal point. It is the great deepness of focal point which makes SEM superior to TEM for certain applications.

Atomic Force Microscopy ( AFM ) : AFM is used to qualify surfaces of crystalline and formless, biological, man-made merchandises including crystals and movies and besides to qualify the microstructure of silicon oxide.

Surface chemical science word picture:

On the solid surfaces such as inside of micro pores, spacial suppression, other equilibrium conditions, other chemical reactions may obtain. Chemical reactions are really of import tool for qualifying solid surfaces. The output will be good compared to the different merchandises. To find the silanol groups with lithiumaluminiumhydride ( LiAIH4 ) , a sample of silicon oxide is degassed in a vacuity and reacts with LiAIH4 at room temperature, the H determined volumetrically. By the other method sample reacts with an alkyl Li or alkyl Mg reagent followed by volumetric finding of the ensuing methane series. After this reaction farther reactions are done with chlorosilanes, intoxicants, BCl3, AlCl3 or hexamethylendisilazane.

Spectroscopic Word picture:

Different spectrometries are used to analyze silicon oxides such as

Nuclear Magnetic Resonance Spectroscopy ( NMR ) :

It is easy to happen the milieus on the Si atom by O atomsand hydroxyl group. The ratios of detected signals are correspond to the proportion to the assorted silica milieus in the sample. It is possible with solid NMR method to ti separate the three chief groups of silicon atom such as

Siloxane Bridges holding chemical shift about 110 ppm

Isolated Terminal SiOH groups holding chemical shift about 100 ppm

Geminal SiOH holding chemical shift about 90 ppm

Infrared spectrometry ( IR ) :

IR is the method for distinguishing between distinguishing between assorted silanol groups. These groups are detected with IR sets in the spectrum are

Isolated SiOH at about 3745 cm-1

Vicinal SiOH at about 340 cm-1

Water bridges about at 3420 cm-1

Thermo analytical methods:

Thermal analysis is given to a group of methods that measure physical belongings of a substance. By differential thermic analysis ( DAT ) it is possible tomonitor the alterations in heat content of a sample while at the class of temperature plan. Thermogravimetry ( ( TG ) and DTA both records the weight loss of the sample as a map of the temperature. By this weight loss information can be obtain on the possible class of debasement. Combination of DTA and TG are used to mensurate the effects of silicon oxide because thermic effects observed in DTA are negligible.

It is besides hard to do decisions sing the construction of a silica surface from the combination of DTA and TG entirely.

X-Ray Diffraction:

Man-made silicon oxide is formless. Silica non possesses three dimensional long range order like crystalline solids. X-ray diffraction method is non possible. Silica countries of short scope order that can be determined by the rating of diffuse X-ray sets. Merely in short scope order these samples can be detected as low 200 grade centigrade utilizing X-ray diffraction.

Loss on drying:

Loss on drying and loss on ignition are holding of import characteristic parametric quantities that can be used to qualify the difference between silicon oxide. Precipitated silicon oxide and silicon oxide gels typically present a loss on ignition of more than 3 % .4


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Figure 2: Ibuprofen construction 6

Name: Ibuprofen

Synonym: : 2- ( 4-isobutylphenyl ) propinoic Acid, 4-Isobutyl-Alpha-


Mol expression: ( CH3 ) 2CHCH2C6H4CH ( CH3 ) COOH

Mol.Wt: 206.29

Melting point: 74 -770 C

Solubility: Partially indissoluble

Ibuprofen ( C13H18O2 ) was foremost discovered by Dr. Stewart Adams in United Kingdom with his co-workers. The chemical name of isobutylphenyl propionic acid is 2- ( 4-isobutylphenyl ) propanoic acid, which is an organic compound in the derived functions of Propionic acid.7

Ibuprofen holding two mirror images signifiers which is a chiral molecule. Due to its structural formation no demand to trouble oneself for dividing enantiomorphs in the isobutylphenyl propionic acid incorporating formulations.8

Ibuprofen is chiefly known for its NSAID ( non steroidal anti-inflammatory ) belongingss by suppressing active enzyme known as cyclo-oxygenase named as COX. These COX enzymes suspected to be suspected two more enzymes subsequently by researches they found its true and recognised as COX-1 and COX-2 materialised. So that they recognised COX-1 is present in all degrees of the organic structure in all conditions because it is a consistent enzyme. Therefore the side effects arose from suppression of the consistent COX-1 enzyme, and by suppressing COX-2 enzyme it is holding benefits therapeutically.7 The chief mechanism is when the COX enzymes converts in to fatty acids to prostaglandins, at the terminal of the concatenation it reacts with COX enzyme so it causes hurting, febrility and redness. So Ibuprofen inhibits this concatenation and gives relief.8

1.3.1 ) Ibuprofen uses:

Chiefly isobutylphenyl propionic acid is used as an NSAID. It is besides used as analgetic. It is used to handle concerns, backaches, athletic hurts, dental pain.9

1.3.2 ) Side effects:

Ibuprofen drug disturbances stomach and causes sickness, purging. It besides causes irregularity, concern, diarrhea, giddiness. It may do serious liver disease. It shows some allergic reactions such as itchiness, roseola, swelling, problem breathing.10


Delivery of a pharmaceutical drug in to the systemic circulation, and Acts of the Apostless on the site of action to bring forth its pharmacological consequence, is the concluding consequence of Drug delivery.11


Figure 3: Flow chart representation of drug bringing 12

In a biological system, different mechanisms are located to protect the system from the foreign substance while continuing alimentary consumption. The physiological agreement and the biological and the chemical barriers associated with the constructions from the first line of the unconscious defense mechanism procedure. If the drug delivered from any path, will about hit and do an impact of these physiological and chemical barriers before making the site of action.

Physiological barriers:

The GI piece of land is bounded with an aqueous mucous secretion bed which is secreted by the goblet cells. The thickness of the enteric mucous membrane varies from 100 to 150 um. Mucus bed Acts of the Apostless as filter for molecules holding molecular mass 600-800 Daltons. After this procedure it entered in to columnar epithelial cell connected together by intra cellular junctions. These beds of the cells are composed of goblet cells, enterocytes, paneth cells. The Epithelial bed is in vigorous contact with the lms of the gastro enteric piece of land. The muscularis mucous membrane makes up the deep bed, which is thought to be interfering in contractility. By these stairss a drug can over take the enteric mucous membrane through several mechanisms depends on physicochemical properties.12

Chemical barriers:

The solubility and its permeableness profiles are determined by its chemical construction. For the rate and extent of soaking up, the concentration at the enteric lms and the pervasion of the drug through the enteric mucous membrane are responsible.

It is believed that metabolic stableness and permeableness of a drug molecule are two chief factors in drug bringing of a drugs soaking up when the solution holding molecule.12



All the experiments discussed here.

2.1 ) Chemicals and Materials:

These chemicals and reagents are used in all over the procedure.

Name of the Chemicals

Beginnings of the Chemicals


Sigma Aldrich Chemical GMbH, Product of India.

Ethyl alcohol

BDH Laboratory Supplies, England. Poole prode-28304. Ec label figure: 20057806.


Fisher Scientific UK Limited, Fisher: 880, code-A/3240/PB17. Batch: 0804270

3-aminopropyltriethoxy silane

Sigma Aldrich Chemistry, 99 % . Cat:440104, Lot no: 92196EJ-259


Sigma Aldrich Limited. Gillingham-Dorset. SP8 4XT-UK. Lot figure: 200681720


Fisher Scientific UK Limited. Code: T/2250/17, Batch: 0942848

Methyltriethoxy Silane

Merchandise of US, 97 % . Code: 250540500, CAS: 1185-55-3, EC- 214-685-0, Lot: A0210064.

2.5 M HCL Solution

Fisher Scientific Limited. Batch: 0934592, Code: U/1150/P1317. S.G- 1.8 ( A¬36 % )

Distilled H2O

Made in the Link Lab Laboratory. University of Greenwich, UK.

Sodium dodecyl sulfate

C12H25O4SNa, mol wt- 288.4, L-6026, SIGMA ULTRA.

Tween 20

A PROD CODE: 13 70 9084, CAS: 9005-64-5,

Merchandise of UK SIGMA ALDRICH.

Table 2: List of chemicals

2.2 ) Equipments used:

Different Equipments were used to establish the optical density and Surface country. Such as

2.2.1 ) Ultra violet/Visible spectrometry:

Ultra violet spectrometry is used to happen the drug consumption and drug release of the given sample. The prepared samples were examined in Shimadzu UV spectrometry. SDS, Tween20, Ammonia are observed at 264nm.

2.2.2 ) Surface country:

The Surface country of silicon oxide prepared by SDS, and Tween 20 and Ammonia which are loaded by Ibuprofen drug are is determined by nitrogen surface assimilation utilizing the BET method on micrometrics Gemini surface country analyzer.

2.2.3 ) Freeze drying: 13

The freeze procedure contains of stop deading the stuff. In a research lab, this is frequently done by puting the stuff in a freeze-drying flask and revolving the flask in a bath, called a shell deep-freeze, which is cooled by mechanical infrigidation, dry ice and liquid N. On a larger-scale, freeze is normally done utilizing a freeze-drying machine. It is importantA A to chill the stuff below its eutectic point, the lowest temperature at which the solid and liquid stages of the stuff can coexist. This ensures that sublimation instead than runing will happen in the undermentioned stairss. Larger crystals are easier to freeze-dry. To bring forth larger crystals, the merchandise should be frozen easy or can be cycled up and down in temperature. This cycling procedure is called tempering. However, in the instance of nutrient, or objects with formerly-living cells, big ice crystals will interrupt the cell walls. Normally, the freeze temperatures are between -50 A°C and -80 A°C. The freezing stage is the most critical in the whole freeze-drying procedure, because the merchandise can be spoiled if severely done.

Amorphous ( glassy ) stuffs do non hold an eutectic point, but do hold a critical point, below which the merchandise must be maintained to forestall melt-back or prostration during primary and secondary drying.

2.3 ) Synthesis of Silica:

Silica was prepared in three signifiers with Sodium dodecyl sulfate, Tween20 and Ammonia by following earlier articles ( 14, 15, 16 )

2.3.1 ) silicon oxide readying with formal South dakota:

Sodium Dodecyl sulfate have chemical expression C12H25NaO4S. SDS is an anionic wetting agent. It is holding a negatively charged sulfonate group for its “ hydrophilic ” terminal and 12- C concatenation for its “ lipotropic ” terminal

Figure 4: Chemical construction of Na Dodecyl Sulfate17


4 gram of Na dodecyl sulfate was dissolved in 32 milliliter of distilled H2O. Then add 64ml of 2.5 M HCL solution and stirred to do homogeneous. Add 9.4 milliliter of TEOS was added to the prepared solution and stirred over dark for 24 hours. This Mixture of solution allow to hoover. The gathered sample is kept in desiccators for a hebdomad. After seven yearss, the sample is dehydrated and 1.07 gram of Hollow mesoporous silicon oxide ( HMS ) was suspended in 50 milliliter of methylbenzene. 0.5446 mmol of Methyl-triethoxy silane was added into the HMS mixture and refluxed at 800C for 48 hours under N2 atmosphere. The obtained solid filtered and by tropic distillment with methylbenzene. For several times HMS give wash with methylbenzene to take H2O. After rinsing the sample it was dried under vacuity at 600C for 2 yearss. Silica was prepared with SDS.

2.3.2 ) Silica readying with Tween20:

Same process used in the 2.3.1. SDS wetting agent was replaced with Tween20 wetting agent. Second batch of silicon oxide is prepared.

2.3.3 ) Silica readying with ammonium hydroxide: Molecular Structure of Ammonia

Figure 5: Ammonia structure18


180ml of Ethanol, 7ml of Ammonia and 50ml deionised H2O were added to a unit of ammunition underside flask. The prepared solution is transferred into a circulating H2O bath which is to be pre-heated to 600C. The solution was stirred at 100 revolutions per minute all over the reaction. If the reaction reaches the temperature, the obtained mixture allowed stable for 2 hours. After which clip 11 milliliter of TEOS was added to originate the precipitate reaction. Further reaction left for 24 hours. To keep the growing of silicon oxide a mixture of H2O and TEOS was added in the ratio of ( 4ml: 24ml ) is added in to mixture in intervals. At the terminal of the reaction a white milky scattering was formed. The reaction was terminated and the scattering set to be cooled. The unreacted ammonium hydroxide and ethyl alcohol removed by centrifugation. Finally silicon oxide was purified by dialysis in deionised H2O at pH 8 and kept for 3 yearss. 3 batches were prepared by the same method and denoted as B1, B2 and B3.

2.4 ) Determination of drug burden and release:

Here the elaborate process of Drug burden and the drug Release was discussed

2.4.1 ) Preparation of standard solution with Ibuprofen -Na:

Standard solution of Ibuprofen Na was prepared to compare with the prepared sample solutions. Stock solution was prepared with 40 mg/ml. 100 milliliter of stock solution was made. By weighing 4 gram of Ibuprofen drug dissolve in 100 milliliter. 1ml, 2 milliliter, 3 milliliter, 4 milliliter and 5 milliliter taken out in equal intervals from the stock solution and dilute with 100 ml H2O.

2.4.2 ) Drug Loading Method:

10 milliliter of Ibu-Na standard solution of concentration 40 mg/ml was added in to 0.25 gram of HMSC at room temperature. This mixture was trasferd in to phials and sealed. These phials are kept for one twenty-four hours. The IBU loaded drug was separated from the solution by osmosis for SDS and Tween20 samples. From prepared two samples, 1ml, 2ml, 3ml was transferred in to 100 milliliters volumetric flask and dilute with distilled H2O up to the grade. This sample analysed by UV /Visible spectrometry at a wavelength of 264 nanometers by taking a little sum of solution into a cuvvet. The obtained Absorbance is compare with the standardization curve for the concentrations.

For Ammonia samples B1.B2 and B3 Loding of IBU-Na was same as the above process and maintain for two hebdomads. For this samples Drug loaded samples seperated with centrifugation at 4000 revolutions per minute. From this 1ml, 2ml, 3ml was transferrd in to 100 milliliters volumetric flask and dilute with distilled H2O up to the grade. This sample analysed by UV /Visible spectrometry at a wavelength of 264 nanometers by taking a little sum of solution into a cuvvet. The obtained Absorbance is compare with the standardization curve for the concentrations.

2.4.3 ) Drug Release Method:

Drug loaded samples were compressed in a tablet compressor with a 100 millimeter diameter and 0.5 millimeter thickness ( approximetly ) . Drug charged tablets are allowed to soak in 100 milliliter of H2O. Temperature maintained at 310K. Sample were taken out for every 5 min with a syringe holding filter paper of 0.20 m and replace after acquiring reading. Measure the absorbence at 264 nanometers utilizing UV/Visible spectrometry for samples SDS, Tween20, B1, B2 and B3

2.5 ) Charecterization method:

Silica charecterization has done merely by Surface country analyzer. By utilizing liquid N sample was filled in to a sampling tubing and given the information and the bonding of liquid N withsolid surface should be strong.19

Chapter – 3


3.1 ) Calibration curve:

With the prepared 40 mg/ml solution different volumes of soutions took and diluted for 100ml H2O

So that, 1 milliliter of stock solution contains = ( 4×1/100 ) gm/ml = 0.04 gm/ml of IBU-Na 2 milliliter contains = ( 4×2/100 ) gm/ml =0.08 gm/ml of IBU-Na 3 milliliter contains = ( 4×3/100 ) gm/ml = 0.12 gm/ml of IBU-Na 4 milliliter contains = ( 4×4/100 ) gm/ml = 0.16 gm/ml of IBU-Na 5 milliliter contains = ( 4×5/100 ) gm/ml = 0.20 gm/ml of IBU-Na

This 1 milliliter, 2 milliliter, 3 milliliter, 4 milliliter and 5 milliliters were transferred in to different 100 milliliter volumetric flask and dilute with H2O upto the grade. So each diluted standard solution contains 0.04 gram, 0.08 gram, 0.12 gram, 0.16 gram, 0.20 gram of IBU-Na

In 1 milliliter, standard solution contain ( 0.04/100 ) gm/ml

So, 1 illuminated standard solution = ( 0.04×1000/100 ) gm/lit = 0.4 gm/lit

As 1 lit= 1000 milliliter, 1gm=1000 milligram 20 = 0.4 mg/ml

In the same method the standard concentrations of 2ml, 3ml, 4ml, 5ml are calculated. From that the standard concentrations are 0.4 mg/ml, 0.8 mg/ml, 1.2 mg/ml, 1.6 mg/ml and 2.0 mg/ml.

For IBU-Na, 264 nanometer is the I»max. By utilizing UV/ Visible spectrometry at 264 nanometer for the standard solution and standardization curve is recorded.


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