Experiment for Identification of Paracetamol

Experiment for Identification of equalityacetamolPATRICK ANTWI MANUIDENTIFICATION OF PARACETAMOL THROUGH THE USE OF PHARMACOPIEA TESTABSTRACTParacetamol is wide used (NHS Choice, 2012) for the relief of tiddler pain, toothache, headaches, symptoms of cold and reduces of patients temperature (control fever symptoms). It is classified as a mild analgesic agent.The following procedures were used during the prove of identification of paracetamol. tender loving care method is important for separation of mixture. This technique is commonly used to determine the comportment of particular escalate through comparison of Rf sets of both unknown precedents and the pattern samples.Melting point analysis is also useful for identification of compound. The thaw point range can be indicated and recorded with the help of a thermometer. For instance, the melting point of paracetamol ranges from168 to172 degree CelsiusInfra-red spectrometry is one of the most essentially useful methods for i dentification of compound. It is usually used to break medicines that contain correct drug in most pharmaceutical industries. Structural information about the functional group of unknown compounds can be discovered through the use of infra-red spectroscopy.Significantly, the results generated during this experiment attest the accuracy and importance of these methods for identification of compounds. For example, the Rf values of tender loving care method as well as infra-red spectroscopy analysis demonstrated the forepart of paracetamol and cafeine in sample B and D respectively.INTRODUCTIONParacetamol is the best alternative choice for children and ulcer patients who have a minor pain such as headache and children. Consequently, too much it (NHS Choice 25/06/2012) can cause severe harm to the kidney and the liver.AIM OF THE EXPERIMENT find out paracetamol from various unknown samples through pharmacopeia test.HypothesisThe range of melting point of the samples that contain parace tamol would be (168 to 172) degree Celsius.Again, the samples that contain paracetamol only would turn into purplish without changing to red after the experiment D.The Rf values of unknown samples that contains paracetamol would be the same as the Rf value of the standard sample when compared. utensil used for the experimentMicro-spatulaUV-lightIndicatorIR spectroscopyMelting apparatusPencilRuleChromatography storage tankTLC plateThin capillary subwayConical flaskBeakerMicro-pipetteMaterials usedEthyl acetateFour unknown samplesWaterDichromateMETHODSMelting point analysisMelting point analysis was conducted for all the four unknown samples labelled A, B, C, and D. Small amount of crystals of each unknown samples was fetched into the melting point capillary tube. The capillary tube contained the sample was primed(p) into the melting point apparatus. The samples temperature was measured with digital thermometer. Hence, both initial and final melting point of the samples was observ ed and recorded. This experiment was repeated 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 located on the mouth of the IR spectroscopy and scanned. The wavelength notice 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 concentrated hydrochloric acid was added to it. The resolving was gently shake and heated to toil for about three minutes. 1ml of water was 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 so lution of potassium dichromate was added to it and the people of colour developed for sample B was violet without changing into red. However, the colour developed 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 solvent system of about 20ml of ammonia methanol chloroform (11980) was placed into the chromatography tank. A filter paper was placed against the wall inside the chromatography tank. The tank lid was placed on to prevent the evaporation of the solvent. The tank was left for about twenty minutes to allow saturated atmosphere to be formed.TLC method was conducted by using 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 acet ate.Moreover, TLC plate was prepared by measuring 1.5cm distance from the brim of the plate with a rule. A horizontal inventory 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 different 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 gradually through capillary action. Hence, the solute spotted on the TLC plate moved up along with the solvent (thus, mobile phase). TLC plate was removed from tank when the solvent reached about 2cm dist ance to the keenness 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 around the new spots formed on the plate. A metre of the distance travelled by both solvent and substance were recorded. The Rf value was careful 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 RANGE171- 175171 172200 206159The sample A is a bit higher than the normal range of the standard paracetamol sample. Equally, sample B indicated the presence of pa racetamol as the ranges 171-172 degree Celsius(c). (d). EXPERIMENT D FOR IDENTIFICATION ANALYSIS resultsSAMPLESABCDColour of solutionSlightly red and turned to purpleVioletYellowish hintDilute violetSample 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 functional groupFrequency / wave number absorptioncm-1Intensityv N-Hamine3319.12 stretchstrongv C-H2794.94 stretchstrong/mediumv O-HHydrogen bond in alcohol, phenol3109.51 stretchStrongv 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 ind icated 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, 0.64 commingle A, C, and D are less polar since they travelled faster and further in the mobile 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 addition, 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 corroborate 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). usable at http//www.nhs.uk/Conditions/Painkillers-paracetamol/Pages/Introduction.aspxAPPENDICESMobile phaseRf value retention factor for thin layer chromatography.Stationary phaseTLC thin layer chromatographyUV light ultraviolet light