Resolve what is requested in the end. Fluocinolone Acetonide raw material titration technique: Sodium phosphate buffer pH4,4 : Dissolve 7.8g of monobasic sodium phosphate in 900mL of water, adjust the pH to 4.40.1 with phosphoric acid or with sodium hydroxide 10N. Adjust with water at 1000mb and mix. Mobile phase: Prepare a mixture of sodium phosphate buffer pH4.4 and acetonitrile (70:30) and fiter it by a membrane of 0.5m. Internal standard solution: Weigh 22.3mg of Norethindrone and transfer to a volumetric flask of 100mL, dissolve and forge with acetonitrile. Standard preparation: Weigh 15mg of Fluocinolone Acetonide Standard in a flask volumetric of 10mL, dissolve and adjust with acetonitrile and mix. Take an aliquot of 0.5mL and transfer to a 10mL volumetric flask, adjust with acetonitrile and mix. Transfer an aliquok 5mL of this solution, 6mL of internal standard solution, 15mL of water to a flask volumetric of 50mL, take to capacity with acetonitrile and mix. Sample preparation (in duplicate): weigh 15mg of Acetonide raw material Fluocinolone, in a volumetric flask of 10mL, dissolve and adjust with acetonitrile and mix. Take an aliquot of 0.5mL and transfer to a volumetric flask of 10mL, forage with acetonitrile and mix. Transfer an aliquot of 5mL of this solution, 6mL of the internal standard solution, 15mL of water to a volumetric flask of 50mL, take to capacity with acetonitrile and mix. Chromatographic system. The liquid chromatograph is equipped with a detector at 220nm and a column 4mm diameter 30cm long containing particles 3 to 10m packed with L. The flow rate is 2mL per minute. Inject 20uh of the standard preparation and record cesponses of the peaks. The relative retention time is about 0.5 for fuocinolone and 1.0 for Norethindrone. Inject, in duplicate, 20uL of sample preparation and record tesponses of the peaks. 1. Calculations for the Mobile Phase. Knowing that the mobile phase will be handled separately, L.s, in a bottle the phosphate buffer pH4.4 and in another bottie the acetonitrile and that 2 samples will be prepared, injecting each one in duplicate, and the standard will be injected 5 times: a) Calculate the amount of mobile phase ( mL ) that will be consumed by the equipment if each run Analytical lasts 15 minutes. b) Based on the answer above, how much buffer (mL) would you need to filter to put it in the team? How much salt would it weigh to prepare this buffec? 3. Considering the information for year 2 and based on the following results obtained during The performance of the analysis determines the percentage of assessment in each of the samples of Fluocinolone Acetonide raw material and AVERAGE. Standard Data Weight: 15.5mg Strength: 98.97% flucinolene area 758720 Internal Standard Area =9489 Sample 1 data Weight: 15.3mg : Elucinglons area =749736 internal Standard Area =9298 Weight: 15.5mg; Flucinolone area =787841 Internal Standard Area = 9587 Sample 2 data
