Quantitation by Extraction

Quantitation by ExtractionSyed Masood Hassan Akbari unveilingA liquid-liquid extraction strain consists of a component (a) which is to be remove from the gift phase. The addition of a second phase (b) a response phase which is immiscible with the feed phase but the component (a) is alcohol-soluble in both the feed phase and the solvent phase. As it happens the solute (a) is transferred from the feed phase to the solvent phase. After extraction the feed and solvent phases atomic number 18 called the raffinate and the extract phases respectively.Usually one of the twain phases is an ingrained phase composition the other is an aqueous phase. Under equilibrium conditions the distribution of the solute (a) over the cardinal phases is determined by the distribution law. After the extraction the two phases sewer be discriminate because of their immiscibility. Component (a) is because separated from the extract phase by distillation and the solvent is then regenerated. Further e xtractions may be carried out to remove more of the component (a).Once the product of recreate has been extracted finally an absorbance reading can be found at its alike max. prefigure 1 Shows the chemical substance structure of trimethoprim.Figure 2 Shows the chemical structure of sulfamethoxazole.This experiment consisted of three main componentsThe quantification of trimethoprim and sulfamethoxazole in a suspension of Septrin.Interpreting the data ga in that locationd and utilize it in collusive the content of trimethoprim in Septrin.Interpreting the data gathered and using it in calculating the content of sulfamethoxazole in Septrin.EXPERIMENTALExtraction of trimethoprim and sulfamethoxazole from SEPTRIN.Figure 3 Illustrates a schematic of the entire extraction mapping consisting of trimethoprim and sulfamethoxazole in SEPTRIN oral solution.sulfamethoxazole (Standard, Sample and Blank prep)Figure 4 Illustrates sulfamethoxazoles sample preparation.The standard was prepared i n the engage manner in a 250ml volumetric flaskful with using 0.2g of sulfamethoxazole in 50ml 0.1M NaOH and topping up with water. The functioning to follow was the exact similar as the sample prep.The blank was prepared in the same manner and water was utilize along with the re ingredients outlined above in sample prep.Trimethoprim (Sample and Blank prep)The already extracted bottom floor with chloroform was extracted once more using four 50ml quantities of 1M acetic acid and the top layers were combined and serve with 5ml chloroform and the top layer added to a 250ml volumetric flask and modify with 1M acetic acid to the mark. 10ml of this solution was then added to a nonher 100ml volumetric flask and 10ml of 1M acetic acid was also added and topped up with water.The blank was make by using 0.2M acetic acid solution.RESULTSDetermining the quantity of trimethoprim and sulfamethoxazole in an oral suspension of SEPTRIN.Table 1 Shows the absorbance values obtained at each re spective max for trimethoprim and sulfamethoxazole.CalculationsTrimethoprimThe sample had a dilution factor of 1 atomic number 19 which meant that there were two dilutions carried out where the suspension was diluted to 250ml, which is a 1100 dilution. Secondly the sample was diluted too 100ml, which is a 110 dilution. These two dilutions steps combined gave a 11000 dilution factor. The calculations were carried out as below.2.5ml in 250ml1100 (Dilution ratio)110 (10ml in 100ml)Therefore 11000 dilution factor.Absorbance 0.332 x 1000 = 332A1%/1cm=204 so 1% solution has 204 absorbance1%conc = 204X = 332332(1)/204 = xX= 1.627% w/v It complies with the complaisance demarcation line of (1.44-1.76)% w/v.Sulfamethoxazole0.2g in 250ml200mg in 250ml (1100 dilution ratio)0.8mg in 1ml (150 dilution)0.016mg in 1ml (110 dilution)0.0016mg in 1mlSample of sulfamethoxazole absorbance = 0.075So, 0.0016mg in 1ml = 0.293And, x = 0.0250.0250.0016/0.293 = xX = 0.0001365mg in 1ml0.0001365mg in 1 ml x 5 0000 = 6.826mg in 1ml6.826mg in 1ml 0.06826g in 1ml 6.826g in 100mlX = 6.826% w/v It does not comply with the compliance limit of (7.4-8.6)% w/v.Trimethoprim and SulfamethoxazoleThe concentration of trimethoprim and sulfamethoxazole in 5ml of SEPTRIN were calculate as shown below.Trimethoprim 1.627% 1.627g in 100mlSo, x in 5ml100x = 8.135gX = 0.08135g in 5ml SEPTRINSulfamethoxazole 6.826% 6.826g in 100mlSo, x in 5ml100x = 34.13gX = 0.3413g in 5ml SEPTRINCONCLUSIONThe lively ingredients in SEPTRIN, trimethoprim 1.627% w/v and sulfamethoxazole 6.826% w/v were segregated by extraction. The concentrations of trimethoprim and sulfamethoxazole in the 2.5ml suspension were calculated to be as stated above respectively. The content of trimethoprim fell within the compliance limit but for the sulfamethoxazole the content fell a bit niggling of the compliance limit suggesting apparatus malfunction or human illusion in making up sample. Trimethoprim complies with the limit set out on t he BP but for sulfamethoxazole it falls under the limit stated on the BP.QUESTIONSIllustrate the extraction procedure.Support the separating move in a mobilize clamp on a ring stand. Make sure the stopcock of the displace is closed.Place a stemmed funnel in the get along of the separating funnel. Add the liquid to be extracted, then add the extraction solvent. The substance volume in the separating funnel should not be greater than 75% of the funnel volume.Insert a stopper in the neck of the separating funnel. choose up the separating funnel with the stopper in place and the stopcock closed, and make it once gently.Point the stem away from your face and slowly outdoors the stopcock to release some build-up of excess pressure, reclose the stopcock and reduplicate this procedure until only a small amount of pressure is released with it is vented.Shake the funnel vigorously for a minute, release the pressure and then again repeat the step of shaking a few times till there is l ess pressure and the solutes are at equilibrium between the two solvents.Place the funnel back into the ring and let it rest collected until the layers are clearly segregated. While waiting, remove the stopper and place a beaker under the separating funnel.Carefully open the stopcock and allow the lower layer to drain into the beaker. Drain just to the point that the upper liquid however reaches the stopcock.The top layer can be left in the separating funnel if further extractions need to be carried out which do need to be carried out. When finished with the separating funnel store the stopper away from the funnel.Explain why sulfamethoxazole is soluble in the alkaline aqueous solution and trimethoprim is not?It is already known that trimethoprim is classified as a benzylpyrimidine and it protentiates the antimicrobial legal action of sulphonamides eg., sulfamethoxazole. So trimethoprim has a tendency to form insoluble complexes when combined with sulfamethoxazole in alkaline aqu eous media.Write out the chemical reply which leads to the coloured product.The reaction mechanism above shows the coloured dyeing agent N-(naphthalene-1-yl)ethane-1,2-diamine reacting with the diazonium to form the coloured product.Why is ammonium sulphanate added? What would happen if it was forgotten?AMS is used as a reagent to speed up the chemical reaction if it is not included in the reaction before adding the dying agent then the process will either delay in reaching to its finish or not reach it at all.After extraction of sulfamethoxazole, how is the extreme solvent processed?The organic solvent was extracted in four 50ml quantities of 1 M acetic acid. The upper layers were all combined and kept and wash with 5ml of chloroform. The top layer was then dispensed into a 250ml volumetric flask and topped up with 1 M acetic acid. 10ml of this solution was transferred to a 100ml volumetric flask, 10ml of 1 M acetic acid was also added and the flask was topped up with water. A blank was made and the sample from the organic layer was read at 271nm.