In 10 g dried sediment sample added 7 ml 0.2 M NH4Cl solution. A mixture of 100 ml hexane: acetone (1:1) was used as a solvent to extract pesticides with overnight shaking for 12 h on reciprocal or wrist action shaker at 180 rpm. The extract was carefully decanted through activated florisil column (2-3 cm), giving twice wash with25 ml hexane: acetone (1:1) to the sediments. The elute was then washed with 200 ml water and then again aqueous layer was extracted with 50 ml hexane. Finally the hexane layer was washed with 100 ml water and then evaporated to dryness with a vacuum rotary evaporator.
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.
CER Labs 2-3 Figure 1. Friedel-Crafts Acylation. Claim: An acetyl group was efficiently introduced to ferrocene by Friedel-Crafts Acylation (Figure 1). We isolated our crude yield while comparing 2 purification techniques: column chromatography and recrystallization. TLC, NMR, and IR spectroscopy were used throughout the process to identify ferrocene and acetylferrocene in addition to evaluating the levels of purity.
The solid luminol was isolated by vacuum filtration, then its chemiluminescence was demonstrated through its reaction with iron from a solution of potassium ferricyanide. The product obtained was identified on whether it glowed. 6. Data and Results The reaction of the product with potassium ferricyanide produced a blue-green glow. This identified the product as luminol.
3.7 Homogeneous Catalytic reduction of 4-nitrophenol To investigate the redox catalytic activities of the synthesized AuNPs using the olibanum gum, we selected a well-known catalytic reaction the transformation of 4-NP to 4-AP by sodium borohydride (NaBH4) as a model reaction and the reaction was monitored using UV–visible spectroscopy. The absorption peak of 4-NP undergo red shift from 317 nm to 400 nm immediately after addition of NaBH4, corresponding change in the colour of the solution from yellow to intense yellow was observed due to the formation of 4-nitrophenolate ions under alkaline conditions. This peak at 400nm remained unaltered for many days in the absence of AuNPs. This indicates the inability of NaBH4 itself to reduce directly
The crude enzyme was precipitated at 70% saturation of ammonium sulfate, and the protein was collected by centrifugation (10,000×g for 10 min). It was suspended in minimal volume of double-distilled water. The precipitate was dialyzed and used for enzyme purification using column chromatography. The dialyzed sample was loaded on DEAE-cellulose column, which was equilibrated previously with the buffer A (50 mM sodium phosphate buffer, pH 7.4). The column was washed with the five bed volumes of buffer A, and the enzyme was eluted with buffer A
The UV sensitive bands were purified using repetitive preparative TLC followed by crystallization. The identity of Ecdysterone was established by the following procedure: HPLC, with a Shimadzu LC-20, a Phenomenex C-18 reverse-phase Luna C18 which was used with a mobile phase of MeOH:Water (1:1) at 1.80 mL/min and the absorbance was monitored at 254 nm. Studies confirming the presence of a single peak of the isolated Ecdysterone, with a characteristic UV absorption at 246 nm were done using commercial standard Ecdysterone (Sigma) (Figure 2 A and B).
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).
In the round-bottom flask (100 mL), we placed p-aminobenzoic acid (1.2 g) and ethanol (12 mL). We swirled the mixture until the solid dissolved completely. We used Pasteur pipet to add concentrated sulfuric acid (1.0 mL) to the flask. We added boiling stone and assembled the reflux. Then, we did reflux for 75 minutes.