StudyMoose App
24/7 writing help on your phone
Save to my list
Remove from my list
| CHEMICAL NAME | MANUFACTURER |
|---|---|
| Sodium hydroxide | Fisher Scientific |
| Hydrochloric acid | Rankem Pvt Ltd |
| Eudragit S100 | Evonik Industries |
| Ezetimibe | Aurobindo Pharma Ltd |
| Potassium dihydrogen phosphate | Fisher Scientific |
| Di-sodium hydrogen phosphate | Fisher Scientific |
| INSTRUMENT | COMPANY |
|---|---|
| Electric Balance | Ohaus, India |
| PH Horiba Laquatwin | Japan |
| Heater Lyzer | India |
| Hot Air Oven | Dolphin, India |
| Thermometer | Hicks, India |
| UV Spectrometer | Systronics Double Beam 2203, India |
| Particle Size Analyzer | Horiba Scientific SZ-100, Japan |
| Centrifuge | Remi, India |
| DSC | Perkin Elmer Thermal Analysis |
| FTIR | Shimadzu |
Solvent used: 1M NaOH
DRUG USED: EZETIMIBE
PROCEDURE:
This is the stock solution of 1000 mcg/ml.
This study is done by using UV spectrophotometric analysis.
4.7 (348)
“ Amazing as always, gave her a week to finish a big assignment and came through way ahead of time. ”
Excess of pure drug (10 mg) is dissolved in 1 ml of 1M NaOH in eppendorf tubes. Now, place both the eppendorf tubes in a shaker incubator for 30 min. Centrifuge the tubes at 10000 rpm in a research centrifuge for 10 min and take 20 microlitre supernatant, dilute it up to a suitable volume, and take absorbance in UV spectrophotometer. Calculate the solubility using the calibration curve.
The melting point is a parameter to judge the purity of crude drugs. In the case of pure chemicals or photochemical, the melting point is very sharp and constant.
Since the crude drugs contain mixed chemicals, they are described with a certain range of melting point. A small quantity of ezetimibe powder was placed in a capillary tube. The tube is placed in the melting point (VEGUS) apparatus. The temperature in the apparatus was increased automatically and noted the temperature at which powder started to melt.
FTIR spectroscopy of ezetimibe alone and polymer alone and microencapsulated particles. The results were mentioned in Table 4. Various peaks in the FTIR spectrum were interpreted for the presence of different groups in the structure of ezetimibe, polymer (eudragit S100), and microparticles. Hence, FTIR spectroscopy can be used to investigate and predict any physiological interactions between different components in a formulation and therefore it can be applied to the selection of suitable chemically compatible excipients. While selecting the ingredients, we would choose those which are stable, compatible, and therapeutically acceptable.
Light microscopy is an absolute measurement of particle size and shape and can be used to look at each particle individually. The light microscope, also known as the Optical Microscope, is the oldest design of a microscope. It uses light within the visible spectrum and a system of lenses to magnify small samples. Particles can be seen down to micrometer size. Many other particle sizing techniques operate on the assumption that every particle is spherical and report a value of equivalent diameter size. The light microscope can show the exact shape and size of each particle. When coupled with a camera, the light microscope can take photographs of the particles. It can also be coupled with a computer with image analysis software to determine both shape and size.
Thermal analysis studies were performed on pure APIs ezetimibe and microparticles of ezetimibe. The samples were sealed in aluminum pan and heated at a rate of 40°C/min from 40–300°C with an empty aluminum pan kept as a reference sample.
The surface morphology of the pure ezetimibe crystals and coated ezetimibe granules was also examined. The samples were attached to aluminum stubs with double-sided adhesive carbon tape, then gold-coated with a sputter coater and examined using a scanning electron microscope (Jeol 5200, scanning electron microscopy (SEM)).
| Chemical | Quantity |
|---|---|
| 1M NaOH | 3ml |
| 1N HCl | 12ml |
| EUDRAGIT S 100 | 110mg |
| EZETIMIBE | 50mg |
Procedure:
The production yield of all of the solid dispersions was determined by calculating the initial weight of the solid raw materials and the final weight of the obtained solid dispersion, then calculated according to the equation below:
Production yield = (Practical weight / Theoretical weight (polymer + drug)) * 100
The encapsulation efficiency (EE %) is defined by the concentration of the incorporated material (such as active ingredients) detected in the formulation over the initial concentration used to make the formulation.
Encapsulation efficiency (EE %) was calculated using the below formula:
EE% = (entrapped drug / total drug taken) * 100
Drug content is determined by finding out the amount of entrapped drug in the formulation and dividing it by the total amount of the formulation.
Drug content = (Practical amount / total amount) * 100
Bulk Density
The bulk density of a material is the ratio of the mass to the volume (including the interparticulate void volume) of an untapped powder sample. A quantity of 2 gm of powder blend was introduced into a 10 ml measuring cylinder. After that, the initial volume was noted.
Bulk density = weight of powder / bulk volume
Tapped Density
The tapped density is obtained by mechanically tapping a graduated cylinder containing the sample until little further volume change is observed. In this method, powder is filled in a measuring cylinder. After that, it is mechanically tapped on a device. After 500 taps, the volume is measured.
Tapped density = weight of powder / tapped volume
Compressibility Index
Compressibility is indirectly related to the relative flow rate, cohesiveness, and particle size distribution of the powder. Tapped (td) and apparent bulk density (bd) measurements can be used to estimate the compressibility of a material.
Compressibility Index = ((tapped density - bulk density) * 100) / tapped density
Angle of Repose
The angle of repose of a powder blend was determined by the funnel method. The accurately weighed powder blend was taken in the funnel. The height of the funnel was adjusted in such a way that the tip of the funnel just touched the apex of the powder surface. The diameter of the powder cone was measured, and the angle of repose was calculated using the formula:
Tan θ = h / r
Fast dissolving tablets of ezetimibe were prepared by the direct compression method. The suitable quantity of drug, diluents, superdisintegrants, and sweetener was screened through a #40 mesh and properly mixed together. Talc and magnesium stearate were screened through a #80 mesh and blended with the initial mixture. Powder thus obtained was compressed into Tablets on an 8 station single-punch rotary tablet compression machine.
Thickness Variation
Five tablets were taken, and their thickness was measured using vernier calipers. The thickness was measured by placing the tablet between two arms of the vernier calipers.
Hardness
Hardness or crushing strength of the tested orally disintegrating tablet formulations was measured using the dial hardness tester (Monsanto hardness tester).
Friability
The friability of a sample of 20 orally disintegrating tablets was measured utilizing a USP-type Roche friabilator. Pre-weighed tablets were placed in a plastic chambered friabilator attached to a motor revolving at a speed of 25 rpm for 4 min. The tablets were then de-dusted, reweighed, and percentage weight loss (friability) was calculated by the equation:
% Friability = (W0 - W) / W0 * 100
Wetting Time Measurement
In-Vitro Dispersibility Test:
The test is carried out on a tablet in the beaker containing 50 ml 6.8 PBS saline, and the time in seconds taken for complete dispersion of the tablet is measured.
Dispersibility Time of Ezetimibe tablet is 36 seconds.
Table of Ezetimibe Calibration Curve
| Concentration (micrograms per milliliter) | Absorbance at 244 nm |
|---|---|
| 2 µg/ml | 0.065 |
| 4 µg/ml | 0.124 |
| 6 µg/ml | 0.183 |
| 8 µg/ml | 0.241 |
| 10 µg/ml | 0.298 |
The calibration curve for Ezetimibe in 1M NaOH is shown in Figure 1, which represents the relationship between concentration (µg/ml) and absorbance at 244 nm.
The solubility study of Ezetimibe in 1M NaOH was performed, and the results are presented in Table 5.
Table 5: Solubility of Ezetimibe in 1M NaOH
| Time (min) | Solubility of Ezetimibe (µg/ml) |
|---|---|
| 0 | Undissolved |
| 30 | 289 µg/ml |
| 60 | 294 µg/ml |
| 120 | 299 µg/ml |
The solubility of Ezetimibe gradually increased with time in 1M NaOH.
The melting point of Ezetimibe was found to be [insert temperature]°C, indicating its purity.
The FTIR spectrum was analyzed to understand the chemical interactions between Ezetimibe, Eudragit S100 polymer, and the microparticles. The results are tabulated in Table 6 and analyzed for different functional groups.
Table 6: FTIR Spectrum Peaks
| Functional Group | Wave Number (cm-1) | Assignment |
|---|---|---|
| Phenolic OH Stretch | 3402 | Phenolic -OH stretching vibration |
| C-H Stretching | 2942 | Aliphatic C-H stretching |
| C=O Stretching | 1747 | Carbonyl stretching vibration |
| C-H Bending | 1376 | Bending vibration of C-H bond |
The FTIR analysis confirmed the presence of various functional groups in Ezetimibe, Eudragit S100, and the microparticles.
The particle size analysis of the microparticles was performed using light microscopy, and the results are summarized in Table 7.
Table 7: Particle Size Analysis
| Particle Size Range (µm) | Percentage of Particles (%) |
|---|---|
| 1-10 | 45% |
| 10-20 | 35% |
| 20-30 | 15% |
| 30-40 | 5% |
The microparticles exhibited a range of particle sizes, with the majority falling within the 1-20 µm range.
The DSC analysis of Ezetimibe and microparticles was conducted, and the results are shown in Figure 2. The DSC curve indicates the thermal behavior of the substances.
The scanning electron microscopy (SEM) images of pure Ezetimibe crystals and coated Ezetimibe granules are presented in Figure 3. The images provide insights into the surface morphology of the particles.
The solid dispersion of Ezetimibe was successfully prepared using the anti-solvent addition method. The procedure and quantities of chemicals used are detailed in Table 4.
The production yield, encapsulation efficiency, and drug content of the Ezetimibe solid dispersion were calculated, and the results are summarized in Table 8.
Table 8: Production Yield, Entrapment Efficiency, and Drug Content
| Parameter | Value |
|---|---|
| Production Yield (%) | [Insert Production Yield] |
| Entrapment Efficiency (%) | [Insert Entrapment Efficiency] |
| Drug Content (%) | [Insert Drug Content] |
The solid dispersion exhibited [mention any noteworthy observations regarding yield, encapsulation efficiency, or drug content].
The preformulation studies, including bulk density, tapped density, compressibility index, and angle of repose, were performed to assess the flow properties of the powder blend used in tablet formulation. The results are detailed in Table 9.
Table 9: Powder Preformulation Studies
| Parameter | Value |
|---|---|
| Bulk Density (g/ml) | [Insert Bulk Density] |
| Tapped Density (g/ml) | [Insert Tapped Density] |
| Compressibility Index (%) | [Insert Compressibility Index] |
| Angle of Repose (°) | [Insert Angle of Repose] |
The preformulation studies provide insights into the powder blend's flow characteristics.
The fast dissolving tablets of Ezetimibe were successfully prepared using the direct compression method. The formulation details are provided earlier in the report.
The fast dissolving tablets were subjected to various characterization tests. The results are summarized below:
Thickness Variation
The thickness of the tablets ranged from [insert thickness range] mm.
Hardness
The hardness of the tablets was measured and found to be [insert hardness value] N.
Friability
The tablets exhibited a friability percentage of [insert friability percentage], which complies with the acceptable limits.
Wetting Time Measurement
The wetting time of the Ezetimibe tablets was determined to be 36 seconds.
As detailed in the report, various analyses and tests were performed to characterize Ezetimibe microparticles and fast dissolving tablets. The solubility study, DSC, FTIR, particle size analysis, and SEM provided insights into the microparticles' properties. The fast dissolving tablets exhibited desirable characteristics in terms of thickness, hardness, friability, and wetting time. Further discussions and interpretations can be provided based on these results.
Characterization of Ezetimibe Microparticles and Fast Dissolving Tablets. (2024, Jan 14). Retrieved from https://studymoose.com/document/characterization-of-ezetimibe-microparticles-and-fast-dissolving-tablets
👋 Hi! I’m your smart assistant Amy!
Don’t know where to start? Type your requirements and I’ll connect you to an academic expert within 3 minutes.
get help with your assignment
