4- Set up reflux system using a clean and dry condenser . 5- Place the flask on the hot plate and heat the reaction for 45 minutes - 1 hour . 6- When the reflux is over , remove magnetic stirrer and allow the reaction to cool to room temperature . 7- Add 20 ml of ice water to a separating funnel
Acetonitrile at a PH of 7 (neutral) is added to each of the test tube samples. Mix the samples on a vertex shaker for 3 minutes and transfer to a 20 ml centrifuge tube and place in a TurboVap under 5-psi nitrogen at room temperature and allow it to completely dry. The dry resides are now put in 1ml of acetonitrile for testing (analysis). 4. Chromatographic Condition 10ml of the extract is now taken to be analyzed using a mass spectrometer and a liquid chromatograph.
TLC, NMR, and IR spectroscopy were used throughout the process to identify ferrocene and acetylferrocene in addition to evaluating the levels of purity. Evidence: The objective of our experiments was to prepare acetylferrocene from ferrocene. The overall reaction was carried out using 6.1 equivalents of liquid acetic anhydride to 1.8 equivalents of phosphoric acid and concluded with an aqueous workup with NaOH. The initial reaction mixture containing ferrocene, acetic anhydride, and phosphate acid was mixed on a hot stir plate. During this period, reflux was observed, and the mixture appeared dark brown in color.
Complexation techniques(1,13,12) Different methods can be used to transport out the complexation of the cyclodextrin with drug. approximately of which are described lower: 1.4.1. Physical blending/milling/co-grinding: Mechanical energy is used to mixture, mill or co-grind the drug and the cyclodextrin. 1.4.2. Kneading Technique: In this technique Cyclodextrin is initially taken in mortar then drug is gradually further into it and using small percentage of water it is triturated using pestle to get a paste like uniformity.
The solution homogeneity expelled, by centrifugation for 10 min. The sample was centrifuged and separated into two layers, and took the top of the sample is injected for HPLC (11,12). Measured concentration in total lipid: The total fats balanced concentration of the pesticide getting by dividing the measured pesticide residue concentration in the overalll tissue sample by the decimal fraction of the sample that consisted of ether-extractable lipid. The total lipid content of each specimen was estimated from its total cholesterol & triglycerides levels by using a summation method. Analytical results for organochlorine pesticides were reported on a lipid-adjusted basis (nanograms per gram or parts per billion) (14).
4.2 PREFORMULATION STUDIES PREFORMULATION STUDIES Preformulation testing is an investigation of physical and chemical properties of a drug substance alone and when combined with excipients. It is the first step in the rational development of dosage forms. Preformulation commences when a newly synthesized drug shows sufficient pharmacologic promise in animal models to warrant evaluation in man. These studies should focus on those physicochemical properties of the new compound that could affect drug performance and development of an efficacious dosage form. A thorough understanding of these properties may ultimately provide a rationale for formulation design, or support the need for molecular modification.
DMF was used as a solvent and AIBN (0.5% w/w of total monomer) as free radical initiator .The reaction was carried out at 70±2° C for 6 hour with constant stirring. After completion of the process it was cooled to room temperature and resultant polymer solution was poured in the large amount of methanol with stirring when polymer precipitated out. It was filtered and washed with methanol. The polymer was purified by repeated precipitation using methanol from solution in DMF and then it dried. 2.3 Preparation of PS
The final volume was recorded. A pH probe connected through Microlab was calibrated using buffer solutions of pH 4.00, 7.00, and 10.00. The calibrated pH probe was used in order to measure the pH of the titrated solution of the unknown weak acid. These same steps were repeated except 2 mL of the strong base were titrated into the weak acid solution instead of 4 mL. This process was repeated 10 times.
ZPFe (3 mol%) was added to a mixture of a benzoyl chloride (10 mmoL) and an aromatic compound (10 mmoL). The reaction mixture was stirred for the appropriate reaction times at 80 °C (Table 2). After completion of the reaction (monitored by thin-layer chromatography, TLC), the mixture was diluted with Et2O and filtered. The organic layer was washed with 10% NaHCO3 solution and then dried over anhydrous Na2SO4. The solvent was evaporated under reduced pressure and the product purified by column chromatography on silica gel to give the corresponding pure aryl
(2006), after slight modifications. The fundamental principle of the DPPH method is the reduction of the DPPH radical in an ethanolic solution by an H-donator antioxidant (AH) to form the non-radical form DPPH-H. In a microtube, 10 µL of each fraction at different concentrations (10 - 1000 µg/mL) were mixed with 990 µL of a DPPH solution (0.1mM) prepared daily. The reaction was allowed to develop for 30 minutes in the dark at room temperature, and then the absorbance was read at 515 nm with a spectrophotometer (Spectronic Helios Alpha UV-Visible, Thermo Electron Corporation, U.S.A). The analysis was done in triplicate for each