4A.2.9.2. Differential Scanning Calorimetry (DSC): DSC analysis measures the heat loss or heat gain resulting from physical or chemical changes within a sample as a function of temperature. DSC analysis was carried out to study the polymorphic transitions exhibited bythe SLN formulation. It was carried out for pure drug, bulk lipids L2 and L3 and the two lyophilized formulations. Thermal behavior of the developed formulation was studied using a differential scanning calorimeter (Universal TA Model Q 200). About 5mg of sample was placed in 50µL Fig 4A.9 DSC thermogram of Pure Drug perforated aluminium pans and sealed. The sample was purged with pure dry nitrogen at a flow rate of 50 ml/min. DSC scan was carried from 0-300 0C at a heating rate …show more content…
no. 4A.13: DSC thermogram of Lipid 3 Fig 4A.14: DSC thermogram of Batch B Fig 4A.15: Integrated DSC Curves of Drug, Lipid 3and Formulation B 4A.2.9.3. X-ray Diffraction (XRD): XRD analysis was carried out to study the degree ofcrystallinity of the drug, lipids and the formulations. Studies were carried out using Philips Expertpro MPD diffractometer (PAN Analytical Inc Germany) with resolution of 0.001Aº. Vacuum grease was applied over the glass slide to stick the sample. About 10 mg of sample was sprinkled over to make a layer having a thickness of ~0.5 mm. The samples were radiated using a Cu target tube and exposed to all lines (λ-1.54056). Scanning angles ranged from 5º to 40º of 2θ. The current used was 30mA and voltage of 40kV. XRD analysis was carried out for the pure drug, physical mixture of drug with each of the lipids (L2 and L3) and the two lyophilized batches (AL and BL). Drug peak has disappeared in XRD of Nanoparticle 3 which probably may be due to conversion of Tamoxifen citrate from crystalline state to amorphous state or dissolution during the heating involved in the preparation of solid lipid nanoparticle or may be another phenomenon is drug may be present in polymeric amorphous phase. (Fig
Craig, D. Q. (2002). Pharmaceutical Applications of Micro-Thermal Analysis. Journal of Pharmaceutical Science, 91(5), 1201-1213.
The aspirin crystals were packed into 3 small capillary tubes to ensure that they are compressed so as to prevent any air gaps. Subsequently, the aspirin crystals that are in the 3 capillary tubes are placed into the melting apparatus and the temperature range was recorded. Since the range is quite far from the theoretical value of 140°C, aspirin's purity attained was low due to impurities present. One potential reason is because of the swift cooling. When the aspirin is left to cool, the crystal lattices will form too rapidly which will surround other molecules thus making the aspirin impure. Another reason could be because the recrystallized aspirin has not dry completely and there might me left over solvent that will affect the temperature range of the aspirin.
Experimental: The experimental procedure outlined in the OU Physical Chemistry Laboratory Manual was followed without any deviations.
Firstly, a burette was taken and rinsed with distilled water. Then it was rinsed using the provided NaOH solution.
The purified unknown had a melting point range, as seen in Table 1, of 135-137ºC. When the unknown was combined with acetanilide, the melting point range of the mixture was much lower, at only 97-106ºC. The literature melting point of acetanilide is 114ºC where the literature melting point of phenacetin is 135ºC. When the unknown was combined with phenacetin, as seen in Table 1, the melting point range of the mixture was very close to that of the purified unknown, 134-138ºC, and the literature value of phenacetin. It could therefore be concluded that, based on the solubility and melting point of the unknown component, the unknown could be identified as
In this case study, our concern goes for the chitosan nanoparticles; firstly nanoparticles are able to adsorb and/or encapsulate a drug, thus protecting it against chemical and enzymatic degradation. Furthermore the encapsulated drug may be prevented from crystallization, thus forming a solid solution. Depending on drug solubility in the carrier, a drug load varying from only a few percent up to 50%] Secondly, chitosan is ...
Materials and Methods: An ion exchange chromatography column was obtained and set up for purification with the addition of 0.5 ml ion exchange matrix. 1 ml
Solubility is based on the highest-dose strength of an immediate release product. A drug is considered highly soluble when the highest dose strength is soluble in 250 mL or less of aqueous media over the pH range of 1 to 7.5. The volume estimate of 250 mL is derived from typical bioequivalence study protocols that prescribe administration of a drug product to fasting human volunteers with a glass of water. A drug substance is considered highly permeable when the extent of intestinal absorption is determined to be 90% or higher. Otherwise, the drug substance is considered to be poorly permeable. (Yu et al., 2002)
After the water, has been boiling for 10 minutes, and the temperature inside the test tube has been stable for 5 minutes, record the temperature and remove the thermometer.
Weight of the crystallized acetaminophen (MW = 151.2) the percentage yield was calculated. This calculation was based on the original amount of p-aminophenol used at the beginning of this experiment. Melting point of products was determined and comparison of the final product with that of the crude acetaminophen was carried out. Also compared was the colors of the crude, decolorized, and pure acetaminophen. Pure acetaminophen melts at 169.5 -171°C.
Discuss the possible drug and excipient-related constrains of the formulation (no identity of the drug was given to you at this
About 1 gm. coarse powder was weighted and transferred to a 500 ml conical flask containing 100 ml of water. It was maintained at moderate boiling for 30 minute on water bath. It was cool and filtered in to a 100 ml volumetric flask. Volume was diluted by adding sufficient amount of water. The decoction was poured in test tube, and then shaken in a lengthwise motion for 15 seconds. They were allowed stand for 15 minutes and the height of foam was measured to determine the foaming index.
As we discussed above that pharmacokinetic and pharmacodynamics can be seen as two sides of the same coin in order to gain better understanding of their efficacy and safety profiles.” Generally it is possible to make fairly robust predictions of the pharmacokinetic profile in man using in vitro systems and preclinical pharmacokinetic studies. A previously published survey on the causes of failure in drug development indicated that inappropriate pharmacokinetics were a major cause such as; factors as low bioavailability due to high extraction or poor absorption characteristics, short elimination half-life leading to short duration of action and excessive variability due to genetic or environmental factors. This observation has led to an increased emphasis on pharmacokinetic input to the drug discovery process throughout the pharmaceutical industry. However, it is important to realise that this may only permit the rejection of compounds to b...
== § Test tubes X 11 § 0.10 molar dm -3 Copper (II) Sulphate solution § distilled water § egg albumen from 3 eggs. § Syringe X 12 § colorimeter § tripod § 100ml beaker § Bunsen burner § test tube holder § safety glasses § gloves § test tube pen § test tube method = == = =
The sample was subjected to steam distillation as illustrated in Figure 1. A total of 50ml of distillate was collected while recording the temperature for every 5.0 ml of distillate. The distillate was transferred into a 250ml Erlenmeyer flask and 3.0 g of NaCl was added. The flask was cooled and the content was transferred into a 250-ml separatory funnel. Then 25.0ml of hexane was added and the mixture was shaken for 5 minutes with occasional venting. The aqueous layer was discarded and the organic layer was left inside. About 25.0ml of 10% NaOH was then added and the mixture was shaken as before. The aqueous layer was collected and then cooled in an ice bath. It was then acidified with enough 6.00 M HCl while the pH is being monitored with red litmus paper. Another 25.0 ml of hexane was added and the mixture was shaken as before. The hexane extract was saved and a small amount of anhydrous sodium sulfate was added. The mixture was then swirled for a couple of minutes then filtered. A small amount of the final extracted was tested separately with 1% FeCl3 and Bayer’s reagent.