Step-III: Synthesis of Cr(II) Complexes: The Schiff's base complexes were synthesized by mixing the Schiff's base (1.5 g) in ethanolic solution of Chromium chloride [CrCl2]. This reaction is refluxed in a waterbath for two hours and their volume were reduced to 70% of it’s original volume and residue was obtained. The coloured product obtained was filtered under suction, washed with ethanol. The product were recrystallized from ethanol. Their yields ranges from 50-55%, the product obtained were light green colour and melting point was 2100C.
Apparatus- Chromatography column: C18 (10 microns particle size), with Guard column Flow rate: 1.2ml/min Pressure: 30-40kgf Wavelength: 326nm Mobile phase: methanol : water (95:5 v/v) Internal standard: retinyl acetate Injection volume: 20µl Procedure for Retinol extraction from serum samples- 1) 100 µl of serum sample and 100 µl of Retinyl acetate were added into 12 X 100mm glass test tubes. Vortex-mixed for 30 seconds. Then, kept them at 4 C for 5 mins. 2) 1mL of hexane was added and vortex-mixed intermittently for 60 sec. 3) Centrifuged at 2500 rpm for 12 mins.
Linoleic acid peroxidation was initiated by the addition of 4 mM FeSO4.7H2O, incubated for 60 min at 37oC and terminated by the addition of 2 mL of ice cold trichloroacetic acid (10% v/v). An amount of 1 mL of thiobarbituric acid (1% w/v in 50 mM NaOH) was added to 1 mL of the reaction mixture, followed by heating at 95oC for 60 min. The reaction sample was read at 532 nm.7 The percentage of linoleic acid peroxidation inhibition activity was calculated using the following equation: % Inhibition = [(AB - AA)/AB] x 100, where AB, absorption of blank sample, AA, absorption of test sample. 2.5.4. Metal chelating activity Briefly, 2 mM FeCl2 was added to different concentrations of test sample and reaction was initiated by the addition of 5 mM ferrozine.
In a 150 mL Erlenmeyer flask with a magnetic stir bar placed 0.25 g of anhydrous sodium hydroxide and dissolved it with 10 mL of methanol. The mix was stirred until all of the sodium hydroxide was dissolved. In a 250 mL beaker placed 5 mL of algal oil. The oil was heated to 60ºC. Added 2 ml of the dissolved sodium hydroxide into the heated oil, immediate the mixture turns cloudy.
The capecitabine solution was added to GNPs dispersal and stirred at 1000 rpm for 30 min. The mixture of capecitabine and GNPs dispersal was incubated for 24 h at room temperature for complete loading of drug on NPs and the centrifuged at 20,000 rpm for 30 mins. The obtained pellet after centrifugation was separated from the supernatant solution and redispersed in deionized water prior to further characterization. The capecitabine concentration in redispersed pellet was determined spectrophotometrically at the λmax value of 240 nm, the percentage loading of capecitabine on GNPs was estimated by following
Montmorillonite K10 (Na+MMT) (Himadia), Ion exchange resin (CDH), sulfuric acid (1.84 g cm-3, 98 wt%; Merck), Dimethyl sulfoxide (DMSO) and methanol were used as recieved. SPEEK Synthesis SPEEK was prepared through the via of sulfonation reaction by using concentrated sulfuric acid at desired temperature. The dried PEEK pellets were ground well with the help of a martter for reducing dissolution time of the PEEK polymer. 5 g of crushed PEEK polymer were added slowly into 100 ml of concentrated sulfuric acid solution under stirring rate about 900 rpm till to reach a dark and viscous solution. Then the degree of sulfonation was controlled by changing the reaction time at constant temperature about 50 ºC[Erce Sengul, Hulya Erdener, R. Gultekin Akay, Hayrettin Yucel, Nurcan Bac, Inci Eroglu, international journal of
Add 75 Ml Conc.HNO3 and heat the flask on a boiling water bath. On heating the flask sugar dissolves in nitric acid and copious evolution of nitrous fumes comes out. Discontinue heating. The reaction subsides in about 20 minutes. Pour the hot solution into a porcelain dish, wash the flask with 15 mL of nitric acid and evaporate the acid solution on a water bath
1.25mL of acetic acid and ferric chloride mixture was added to 2.5mL of the pure extract. Occurrence of blue-green color indicates the presence of glycosides. Test for Saponins. 10mL of distilled water was added to 5 mL of the pure extract the mixture was shaken in a graduated cylinder for 15minutes. Occurrence of layer of foam or bubbles indicates presence of saponins.
This has to be prepared fresh. Procedure : (a) Preparation of calibration curve :(i) Pippet portions of standard NiSO4 solution into 100 ml volumetric flask. Use a series from 50 to 250 µg Ni. (ii) Add 25 ml 1.0 N HCl in 5 ml bromine water. (iii) Cool with cold running tap water and add 10 ml concentrated Ammonium hydroxide.
2. Experimental procedure 2.1. Chemicals and materials Melamine (99%), titanium dioxide with anatase (99.7%), isoniazid (ISN, >99%), isopropanol anhydrous (IPA, 99.5%), 1, 4-benzoquinone (BQ, ≥98%) and ammonium oxalate (AO, ≥99%) were purchased from Sigma Aldrich. The molecular structure and chemical properties of isoniazid are given in Table 1. Sodium hydroxide (NaOH, 99%) and methanol (MeOH, analysis grade) was purchased from Merck Millipore, Germany.