Experiment for Identification of Paracetamol

experimentation for Identification of ParacetamolPATRICK ANTWI MANUIDENTIFICATION OF PARACETAMOL THROUGH THE apply OF PHARMACOPIEA TESTABSTRACTParacetamol is widely apply (NHS Choice, 2012) for the relief of minor pain, toothache, vexations, symptoms of frigorific and trigger-happyuces of patients temperature (control fever symptoms). It is classified as a easy analgesic agent.The following procedures were used during the experiment of identification of paracetamol. tender loving cargon order is important for separation of mixture. This technique is commonly used to determine the battlefront of particular heterogeneous by dint of comparison of Rf abide bys of both(prenominal) alien models and the measure ideals.Melting spot analytic thinking is also utilitarian for identification of compound. The resolve point range can be indicated and preserve with the help of a thermometer. For instance, the melting point of paracetamol ranges from168 to172 degree CelsiusInfra- red spectrometry is sensation of the most essentially useful methods for identification of compound. It is usually used to grade medicines that contain correct drug in most pharmaceutical industries. geomorphological information or so the functional group of unknown compounds can be ascertained through and through the use of infra-red spectroscopy.Significantly, the results generated during this experiment attest the accuracy and greatness of these methods for identification of compounds. For example, the Rf set of tender loving care method as rise up as infra-red spectroscopy compendium demonstrated the presence of paracetamol and cafeine in ideal B and D respectively.INTRODUCTIONParacetamol is the best alternative choice for children and ulceration patients who have a minor pain such as headache and children. Consequently, too much it (NHS Choice 25/06/2012) can cause prankish harm to the kidney and the liver.AIM OF THE EXPERIMENTIdentify paracetamol from various unkno wn examples through pharmacopeia test.HypothesisThe range of melting point of the samples that contain paracetamol would be (168 to 172) degree Celsius.Again, the samples that contain paracetamol only would turn into violet without changing to red after the experiment D.The Rf values of unknown samples that contains paracetamol would be the homogeneous as the Rf value of the standard sample when compared.Apparatus used for the experimentMicro-spatulaUV- well-fixedIndicatorIR spectroscopyMelting apparatus drawRuleChromatography armoured combat vehicletender loving care home scale of measurementThin capillary thermionic tubeConical flaskBeakerMicro-pipetteMaterials usedEthyl acetateFour unknown samplesWaterDichromateMETHODSMelting point abridgmentMelting point analysis was conducted for all the quaternity unknown samples labelled A, B, C, and D. Small add of crystals of all(prenominal) unknown samples was fetched into the melting point capillary tube. The capillary tube con tained the sample was laid into the melting point apparatus. The samples temperature was measured with digital thermometer. Hence, both initial and final melting point of the samples was observed and recorded. This experiment was recurrent twice to obtain the ranges of the melting point.INFRA-RED TECHNIQUEDuring the experiment, the arm of IR spectroscopy was cleansed with (ethanol) alcohol. The background of IR spectroscopy was scanned. Hence, each sample was place on the mouth of the IR spectroscopy and scanned. The wavelength detected the various bound in each compound. Copies of each compound scanned was printed out for observation and reading.EXPERIMENT D FOR IDENTIFICATION TEST ANALYSISThe experiment D was conducted for all the four unknown samples labelled A, B, C, and D. 0.1g of each unknown samples were measured with macro spatula and 1ml of strong hydrochloric acid was added to it. The solving was gently shake and heated to boil for about three minutes. 1ml of water wa s added to the boiling solution. After boiling, the solution was then placed in an ice bath to cool. Observation was made and there was no precipitation form. Therefore, 0.05m of 4.9/L solution of potassium dichromate was added to it and the annotate real for sample B was violet without changing into red. However, the color in real for sample A was slightly red and changed to purpled whilst sample C and D developed yellow hint colour and diluted violet colour respectively.TLC METHODA dissolving agent system of about 20ml of ammonia wood alcohol chloroform (11980) was placed into the chromatography ice chest. A filter paper was placed against the wall inside the chromatography tank. The tank lid was placed on to impede the evaporation of the solvent. The tank was left for about twenty minutes to result saturated atmosphere to be formed.TLC method was conducted by apply four unknown samples labelled A, B, C, D and ethyl acetate. During the experiment, a solution was made from each of the four unknown samples A, B, C, and D respectively. Thus, about 10mg of each sample was fetched with micro-spatula into the small beaker and dissolved with the small volume of ethyl acetate.Moreover, TLC plate was prepared by measuring 1.5cm aloofness from the edge of the plate with a rule. A horizontal job was drawn and marked the intervals with a pencil. The distance in between each interval was about 1.5cm apart. The line was demarcated into six intervals for the four unknown samples as well as the standard samples, which comprises of paracetamol and caffeine solution.Each solution was fetched with the help of a micro-pipette and spotted on the TLC plate at distinguishable intervals. In addition, the standard sample solutions of paracetamol and caffeine were spotted on the same plate at different position. Thus, spot A, B, C, D, Par and Caff in that order. The TLC plate was placed into the chromatography tank and covered with the lid. The solvent then moved up gradu ally through capillary action. Hence, the solute spotted on the TLC plate moved up along with the solvent (thus, meandering(a) phase). TLC plate was removed from tank when the solvent reached about 2cm distance to the edge and marked with a pencil.Moreover, the plate was left to dry for about 20 minutes. After the evaporation of the solvent has taken place, TLC plate was then placed under the UV light for observation. A drawing was made with a pencil round the new spots formed on the plate. A measurement of the distance traveled by both solvent and substance were recorded. The Rf value was figure for both unknown samples and the standard samples. Therefore, the Rf value was calculated base on the formula below.Rf value = distance travelled by substance divided by the distance travelled by solvent. Finally, the Rf values of unknown samples were compared with Rf values of the standard samples.The Rf value for paracetamolRf = 3.90/6.1Rf value = 0.639 = 0.64RESULTS(b).Melting point analysis resultsSAMPLESABCDMELTING POINT operate171- 175171 172200 206159The sample A is a bit higher(prenominal) than the normal range of the standard paracetamol sample. Equally, sample B indicated the presence of paracetamol as the ranges 171-172 degree Celsius(c). (d). EXPERIMENT D FOR IDENTIFICATION ANALYSIS resultsSAMPLESABCDColour of solutionSlightly red and rancid to purpleVioletYellowish hintDilute violet take in A developed purple colour which shows para-aminophenolThe colour achieved for sample B was violet which show positive result and it was therefore indicated the presence of paracetamol. The colour developed for sample C was yellow hint which indicated the presence of caffeine. However, sample D developed diluted violet colour which shows the presence of caffeine and paracetamol.Infra-red analysis resultsSample ASample BBond working(a) groupFrequency / wave number absorptioncm-1Intensityv N-Hamine3319.12 stretchstrongv C-H2794.94 stretchstrong/ strong suitv O-HH ydrogen bond in alcohol, phenol3109.51 stretch heartyv C=C1650.71 Aromatic stretchsv C=O1609.82 amide stretchN-H deltaamide1562.66 amide bendv C=CAromatic stretch1504.96 aromatic stretchThe functional group obtained on sample B indicated the presence of paracetamol.Sample CSample D(g). Results for TLC analysisSTANDARD SAMPLESParacetamolCaffeineRf values from TLC analysis0.640.89SAMPLESABCDRf values from TLC analysis0.740.640.890.73The Rf values calculated for TLC analysis indicated that sample B is paracetamol when compare with the standard samples. Thus, 0.64Compound A, C, and D are less polar since they travelled faster and further in the erratic phase and they are more attracted to the mobile phase than compound B.However, compound B is more polar and travel slowly in the mobile phase. It is most attracted to the stationary phase.DiscussionThe experiment D of sample B clearly showed positive outcome and indicated the presence of paracetamol as violet colour was achieved. In addi tion, TLC analysis also indicated that sample B was paracetamol when Rf value of unknown samples compared to the standard samples. Therefore, this shows the accuracy and precision of the positive outcomes of the experiment. Equally, the ranges obtained from melting analysis for sample B also support the presence of paracetamol.Experiment D of sample A showed deep purple colour and the infra-red analysis confirmed that, it is para-aminophenol. Moreover, both experiment D, TLC method and infra-red analysis confirmed the presence of caffeine in sample C.However, sample D developed dilute violet colour TLC analysis which shows a mixture of (two compounds) paracetamol and caffeine. The infra-red analysis also confirmed that, sample D was a mixture of two compounds.TimeSUMMARY REFERENCEBarber, J., Rostron, C.,(2013). Pharmaceutical chemistryHill, G., Holman, J,. (2011) Chemistry in Context. 6th editionNHS Choice, (25/06/2012). Available at http//www.nhs.uk/Conditions/Painkillers-paracet amol/Pages/Introduction.aspxAPPENDICES expeditious phaseRf value retention factor for thin work chromatography.Stationary phaseTLC thin layer chromatographyUV light ultraviolet light