5.1 MATERIAL USED Azathioprine was obtained as a gift sample from M/s Psycorem Pharmaceuticals Ltd. (Ludhiana, India); Carbopol 934 was purchased from Sunchem (India), Tween 20 and Span 20, Methyl and Propyl paraben, Light liquid paraffin, Propylene glycol, Triethanolamine (TEA), and Ethyl alcohol were purchased from M/s Central Drug House Pvt. Ltd ( New Delhi, India). Doubled distilled water was used throughout the study. 5.2 METHOD OF PREPARATION OF AZATHIOPRINE EMULGEL 5.2.1 Preparation of Emulsion The oil phase of the emulsion was prepared by dissolving 0.9 mL of Span 20 in 5 ml of Light liquid paraffin while the aqueous phase was prepared by dissolving 0.6 ml of Tween 20 in 25 ml of purified water. 30 mg of methyl paraben and 10 mg of
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.
Thin Layer Chromatography (TLC) Abstract This experiment uses the TLC chromatography technique to identify the presence of acetylsalicylic and Acetaminophen in analgesic drugs (Tylenol and Anacin). It was found that the Anacin and acetylsalicylic had very closer Rf values (0.8 and 0.79). The Tylenol and acetaminophen had closer Rf values (0.54 and 0.58). Hence, Acetylsalicylic acid and acetaminophen were present in Anacin and Tylenol tablets respectively. Introduction Chromatography is the technique of separating of mixtures based on their intermolecular forces.
5 mL of 3M sodium hydroxide, 5 mL of de-ionized water, and 15 mL of hexane were added to the reaction flask and stirred. The mixture was transferred to a separatory funnel, separated into an organic layer and water layer, and then drained. The water layer was washed twice with 10 mL of hexane. The organic layer was dried
Isolation of Ecdysterone from Sesuvium portulacastrum As detailed in Figure1, Ecdysterone was isolated from Sesuvium portulacastrum using a sequential extraction process with Chloroform (CHCl3) followed by Methanol (MeOH), after which Alumina column chromatography of MeOH extract was performed. The different fractions were then eluted using varying proportions of CHCl3 and MeOH, resulting in MeOH: CHCl3 (20:80) bioactive fraction. Thin-layer chromatography (TLC) analysis of MeOH: CHCl3 (20:80) fraction was carried out using a solvent system containing MeOH (15%) and Ethyl Acetate (85%). The TLC plates were visualized by spraying with vanillin- HCl reagent resulting in a UV sensitive band, which on heating, developed green color. The UV sensitive bands were purified using repetitive preparative TLC followed by crystallization.
The final volume was adjusted with the same solvent to get concentration of 100 µg/ml. the solution was further diluted to get the concentration of 10 µg/ml, filtered through 0.45 µm filter tips , and aliquots of 20 µl from this solution was injected into HPLC by using an
One millilitreer of the lichen extract (1 mg/mL) in a volumetric flask was diluted with distilled water (46 mL), and the content was mixed in a volumetric flask after adding. oOne millilitreer of Folin-Ciocalteu reagent was added and the content of the flask was mixed. thoroughly . After 3 min, 3 mL of 2% sodium carbonate (2 %) was added and then was allowed to standleft for 2 h with intermittent shaking. The reaction absorbance of prepared mixture absorbance was measured at 760 nm in a spectrophotometer (Jenway UK).
The mixture was finally made upto 5 mL with distilled water and placed in hot water bath at 95ºC for 1 h. After cooling, 1 mL of distilled water and 5 mL of the mixture of n-butanol and pyridine (15:1, v/v) was added. The mixture was vortexed and after centrifugation at 4000 rpm for 10 minutes, the absorbance of the organic layer (upper layer) was measured in UV-Vis spectrophotometer (Shimatzu) at 532 nm against blank using distilled water. TBA when allowed to react with MDA aerobically formed a colored complex [MDA-(TBA) 2 complex] which was measured with spectrophotometer. MDA concentration (measured as TBARS) was calculated as
Sample Preparations Unknown water and reagent blanks are prepared in the same manner. 20 ml test tubes are taken and 5ml of water is pipetted into each of the test tubes. The pesticide standards are now inserted into the test tubes at concentrations of 0.1,0.2,1,2,5,10 and 30 ng/ml-1. The mixtures are mixed and kept in equilibrium for 30 minutes. After the 30 minutes is done, the tests tubes are then immersed in a 100 degrees Celsius methanol water bath for 15 minutes.
The purpose of this experiment was to perform a Wittig reaction using two different methods: In method I, 250 mg aldehyde was mixed with 785 mg phosphonium salt in 5 M NaOH solvent. This mixture was stirred for thirty minutes and filter by vacuum filtration for the product. In method 2, 250 mg of aldehyde, 785 mg, benzyltriphenylphosphonium chloride, and 380 mg potassium phosphate tribasic were homogenize with a pestle and mortar. Vacuum filtration was also used in this method to attain the product. The products in both methods were used for recrystallization and TLC.