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Analysis of analgesics and antipyretics.indu


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Analysis of analgesics and antipyretics.indu

  1. 1. 5/4/2013Yalamarty pharmacy college1Presented by…J.N.V. Indira DeviM.Pharmacy 1st yearPharmaeutical analysisYalamarty pharmacy college
  3. 3. ANALGESICS5/4/2013Yalamarty pharmacy college3 • Analgesics are a class of drugs usedto relieve pain by selectivelyinhibiting the perception of the pain.ANTIPYRETICS•An antipyretic is a type of medication thatwill reduce fever by lowering temperaturefrom a raised state.They are available in the form oftablets,capsules,ointments,syrups and parentrals.
  5. 5. 5/4/2013Yalamarty pharmacy college5PARA AMINOPHENOLDERIVATIVES1.Paracetamol,2.AcetophenetidinQUINOLINEDERIVATIVESEx:1.Cinchophen, ,2.NeoCinchophenN-ARYL ANTHRANILICACID/FENAMATESEx: Mefenamic acid ,FlufenamicacidOXICAMS/ENOLICACIDSEx:Piroxicam,IsooxicamSELECTIVE COX2INHIBITORS:Ex: EtoricoxibRofecoxibGOLD COMPOUNDS:EX: Aurothioglucose, aurofin
  6. 6. 5/4/2013Yalamarty pharmacy college6OTHERANALGESICSOpioidsAlpha–2agonistsThiazinederivativesLocalAnalgesics•Morphine•Oxymorphone•Meperidine(demerol)•Methadone•Xylazine•Meditomidine(domitor)•Lidocaine(xylocaine)• Benzocaine
  7. 7. NSAIDsProstaglandinspGE2 pGF2Nerve ending ofpainPainBradykininhistaminefactors+•Analgesic Mechanismblock prostaglandinsproduction• Site of action:peripheral tissueANALGESIC MECHANISM5/4/2013Yalamarty pharmacy college7
  8. 8. NSAIDsPyrogenProstaglandinspGE2thermoregulatorycenterheat production ↑Heat dissipation ↓set point ↑Fever•Antipyretic MechanismBlock prostaglandinsproduction•Site of actionCentralNervousSystemANTIPYRETIC MECHANISM5/4/2013Yalamarty pharmacy college8
  9. 9. METHOD OF ANALYSIS5/4/2013Yalamarty pharmacy college9 Aspirin Diclofenac sodium Aceclofenac Ibuprofen Paracetamol Analgin Antipyrine Indomethacine Mefenamic acid
  10. 10. AspirinMethod of analysisTablet Limits : 95.0 -105.0 % of the stated amount of AspirinUses:-Analgesic and antipyretic.-Anti rheumatic.-Anti gout.-Anti platelet agent.Aspirin is 2-acetoxybenzoic acid.1. Identification:0.5 g drug + 10 ml of sodium hydroxide solution 1.boil for 3 min add 10 ml of dil.sulphuric acid2. coolwhite, crystalline precipitate is producedadd FeClз solution Filter, dissolve the precipitate in2 ml of waterdeep violet colour is produced.
  11. 11. 2.Titrimetric analysisAssay of aspirin.Powdered 20tablets0.5 g ofpowderequivalentdrug taken30.0 ml of0.5 M NaoHadded,gentlyboiledTitrated with0.5 M HCl usingphenol redBlank isperformedEquivalent factor:1ml of 0.5M HCl ≡ 0.04504g of aspirinAmount of aspirin=(B.R-S.R) * volume of NaOH added *(Actual molarity of HCl) * E.FB.R Theoritical molarity of HClB.R=blank readingS.R=sample reading
  12. 12. 3.Chromatographic Method of AnalysisHigh performance liquid chromatography of aspirin Column :C18 silica column (5-um particlesize) Length:25cm Inner diameter: 4.4 mm Flow rate: 1.5 ml/min. Mobile phase :Acetonitrile:Water(HPLC grade)=1:9 Injection volume: 10μl. The detector measures absorbance at 254 nm.Sample Preparation Analgesic tablet was ground into a fine powder Weighed approximately 0.2502g and dissolved in 25 mL of HPLC solventwith gentle heating in a100ml volumetric flask. Cooled to room temperature and diluted to volume with HPLC solvent. Five mL of the solution was diluted to 50 mLwith HPLC solvent ina volumetric flask and injected in to HPLC.
  13. 13. Diclofenac sodiumTablet Limits : 90%-110% of the stated amount of DiclofenacMethod of analysisAlso known as Voltaren SodiumIt ranks Second in sales (1983) world wideIUPAC name:2-{2-[(2,6-dichlorophenyl)amino]phenyl}acetic acidUses:-Analgesic and antipyretic.-In rheumatic fever.1.Identification:0.4 per cent w/v solution in methanol +1 ml of nitric acid dark red colour develops
  14. 14. Assay of diclofenac sodium.2..U.V spectrophotometric methodReference solution : A 1 % w/v solution of diclofenac sodium RS in methanolCalculate the content from the absorbance obtained.Weigh and powder20 tablets50 mg of DiclofenacSodiumShake with 60 ml ofmethanol in a200mL volumetricflaskDilute to volumewith methanolDilute 5.0 ml of thissolution to 100 mlwith methanolMeasure theabsorbance of theresulting solution at285 nm
  15. 15. 3.Potentiometric method by Non-aqueous titrimetry15 End point determined potentiometrically by plotting ∆pH/∆v on y-axis and volumeof titrant added on x-axis. Equivalent factor:1ml of 0.1M HClO4≡0.03181g of diclofenac sodium Amount of drug = volume of titrant consumed * Actual molarity of HClO4 * E.FTheoritical molarity of HClO40.2gm powder equivalent of diclofenactablets+50ml glacial acetic acidTitrate against 0.1M HCl04
  16. 16. Aceclofenac5/4/2013Yalamarty pharmacy college16IUPAC Name:[(2,6-dichlorophenyl)amino]phenylacetoxyacetic acid.Tablet Limits : 99%-110% of the stated amount of AceclofenacUses:-Analgesic and antipyretic.-In rhemuatoid arhritis.Method of analysis1. Identification:When examined in the range 220 nm to 370 nm ,the 0.002 per cent w/v solution inmethanol shows an absorption maximum at 275 nm .
  17. 17. 2.Potentiometric nethod:5/4/2013Yalamarty pharmacy college17Powder 20tablets,take 0.5gpowder equivalentaceclofenacDissolve in 40ml ofmethanolTitrate with 0.1MNaOHBlank is performed.End point is determined potentiometrically by plotting ∆pH/∆v on y-axis and volumeof titrant added on x-axis.Equivalent factor:1ml of 0.1M NaOH≡0.0354g of AceclofenacAmount of drug = volume of titrant consumed * Actual molarity of NaOH * E.FTheoritical molarity of NaOH
  18. 18. IbuprofenTablet Limits : 95%-105% of the stated amount of ibuprofenMethod of analysis1.Identification:Thin-layer chromatography coating the plate with silica gel H.Mobile phase: 75 volumes of n-hexane, 25 volumes of ethyl acetate and 5 volumes of glacial acetic acid.Test solution: 0.5 g of the substance under examination in 100 ml of dichloromethane.Reference solution. A 0.5 per cent w/v solution of ibuprofen RS in dichloromethane.Procedure:• Apply to the plate 5 μl of each solution.• After development, dry the plate at 120 for 30 minutes• Lightly spray the plate with a 1 per cent w/v solution of potassium permanganate in 1 M sulphuric acid.• Heat at 120 for 20 minutes and examine in ultraviolet light at 365 nm.The principal spot in thechromatogram obtained with the test solution corresponds to that in thechromatogram obtained with the reference solution.IUPAC name:2-[4-(2-methylpropyl)phenyl]propanoic acidUses:-Analgesic and antipyretic.-In rhemuatoid arhritis.-In spondilitis.
  19. 19. 2.Titrimetric methodAssay of ibuprofen.Equivalent factor:1ml of 0.1N NaoH≡0.02063g of ibuprofen.Amount of ibuprofen=vol. of NaOH consumed * Actual normality * E.FTheoritical normality3.U.V spectrophotometric methodSolvent: ChloroformWave length:264 nmSo, Ibuprofen present in bulk samples can be estimatedTake 0.2gpowderequivalentdrugExtract with25mL portions ofether andevaporate thecombined etherlayerDissolve theentire residuein 100mlmethanolTitrate with0.1N NaoHusing phenolred
  20. 20. ParacetamolIUPAC name: N-(4-hydroxyphenyl) acetamideUses:-Analgesic and antipyretic.Method of analysis1.Identification0.1 g drug + 1 ml of hydrochloric acid boil 3 minutes add 10 ml of water and coolno precipitate is producedAdd 0.05 ml of 0.0167 M potassium dichromateviolet colourdevelops which does not turn red.
  21. 21.  Reagents:1%w/v 2,4-dinitrobenzaldehyde in 5% v/v 0.1N H₂SO4,1N HCl The schiff’s base measured at 435nm2. Colorimetric method:a)With 2,4-DNBYellowcolour
  22. 22. Reagents: 0.1%w/v solution of sodium nitrite in water. 0.5%w/v solution of ammonium sulpha mate in water 0.1%w/v solution of N-1-napththyl ethylene di amine dihydrochloride(NED) in water. 5N HCLProcedure:b)Diazotization with NED:sample+1mlof 5N HCl1ml of NaNO2soln.mix well for10min inice,below10 cadd 1ml ofammoniumsulphamatethen add 1mlof NEDreagentPink azodye isformedAbsorbancemeasured at555nm.
  23. 23. 3.U.V spectrophotometric method :Assay5/4/2013Yalamarty pharmacy college24 Calculate amount of paracetamol in tablets taking 715 as the specificabsorbance at 257 nm.Powder 20 tablets andWeigh accurately apowder equivalent of0.15g drugadd 50 ml of 0.1 Msodium hydroxide,dilute with 100 mlwatershake for 15 minutesand add sufficientwater to produce200.0 mlMix, filter and dilute10.0 ml of the filtrateto 100.0 ml with waterTo 10.0 ml of theresulting solution add10 ml of0.1 M sodiumhydroxide, dilute to100.0 ml with waterand mix wellMeasure theabsorbance at 257 nm
  24. 24. 5/4/2013Yalamarty pharmacy college25Thin Layer Chromatography Method for the Determination of Paracetamol andIbuprofen in Pharmaceutical Formulation The purpose of this study to obtain an efficient solvent for extractingparacetamol and ibuprofen from sample and a good eluent for separationbetween paracetamol and ibuprofen on the TLC plate. Adsorbant:Silica gel 60 GF 254 . Mobile phase:Ethylacetate : n-hexane, (75 : 25 v/v) Retardation factor (Rf) :Paracetamol: 0.24Ibuprofen: 0.64 Resolution factor between paracetamol and ibuprofen was 6.4. The analyte spots were quantified using densitometry method :Paracetamol:244 nmIbuprofen:260nm
  25. 25. Methods of analysis1.Iodimetry method:Assay1ml of 0.05 M iodine is equivalent to 0.01757 g of AnalginAnalginWeigh accuratelyabout 0.5g powderequivalent ofanalgin from 20tabletsdissolve in a mixture of40 ml of ethanol(95%) and 10 ml of0.01M HCl shake andfiltertitrate 25 ml of filtratewith 0.05 M iodineuntil a yellow colourstable for 30 sec. isproduced.
  26. 26.  Reagents:0.5M Phthalate Buffer: pH:4.00.5%w/v 1,2-napthaquinone-4-sulfanic acid (NQS)-sodium Procedure:2ml of sample add 5ml of buffer + 1ml of NQS-sodiumheat on waterbath for 60 c for 40minextract with chloroformorange colour appearsabsorbance measured at 475nm.2. Colorimetry method:
  27. 27. Method of analysis:1.Gravimetric method2.Colorimetric methods3.Polarographic method IUPAC Name:1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-oneAntipyrineUses:-An analgesic and antipyretic that has been givenorally and as ear drops.-Used in testing the effects of other drugs or diseaseson drug-metabolizing enzymes in the liver.
  28. 28. 1. Gravimetric method The precipitate is weighed to determine the weight of antipyrine present.In a sodium bicarbonatesolution, antipyrine +iodine is addedmono iodo additioncompoundextracted into chloroform+sulphur dioxideIodine released, silvernitrate is addedsilver iodide is pptd.
  29. 29.  REAGENT SOLUTION: P-di methyl amino benzaldehyde (0.5g)is dissolved in a mixture of 4.5ml of concentrated sulphuric acid and8.5ml of water.2.Colorimetric methodPDAB ANTIPYRINE Absorbance measured at 513nmRose redtoSalmon pinkcomplex
  30. 30.  Antipyrine is nitrosated to give a compound which is reducibleat the dropping mercury electrode.Procedure:3. Polarographic method1 ml of 0.1N H2SO4 and 1ml of0.1N NaNO2are added to 1ml ofapproximately 10-2 M antipyrineThe mixture is allowed tostand for 12min at 23 C to28 C, to ensure completereactionExcess HNO2 is neutralizedwith 1ml of 0.1N NaOH0.5ml of 1%gelatin solutionis added, and the solution ispolarographed.Concn. is reported to beproportional to the diffusioncurrent.
  31. 31. Mefenamic acidIUPAC Name: 2-[(2,3-dimethylphenyl)amino]benzoic acid1. Identification:5 mg drug in 2 ml of sulphuric acid + 0.05 ml of 0.0167 M potassium dichromateintense blue colour isproduced immediately which fades rapidly to brownish-green.Method of analysis:
  32. 32. Test solution: Weigh 20 capsules50 mg equivalent Mefenamic acid250 ml volumetric flaskAdd 5 ml of tetrahydrofuranShake for 10 minutes with the aid of ultrasoundDilute with mobile phase & filterReference solution: A solution containing 0.02 % w/v of mefenamic acid RS in themobile phase.2.Liquid chromatography:AssayMobile phase: a mixture of 23 volumes acetonitrile,20 volumes of 0.05 M of monobasicammonium phosphate adjusted to a pH of 5.0 with 3 M ammonia and 7 volumes of THF_ flow rate. 1 ml per minute– spectrophotometer set at 254 nm– a 20 μl loop injector_Inject alternately the test and the reference solution.Calculate the content of C15H15NO2 inthe capsules.
  33. 33. IndomethacinIUPAC Name 2-{1-[(4-chlorophenyl)carbonyl]-5-methoxy-2-methyl-1H-indol-3-yl}acetic acidMethods of analysis1.Identification:Dissolve 0.1 g in 10 ml of ethanol (95 per cent), heating gently if necessaryTo 0.1 ml add 2 ml of a freshly prepared mixture of 1 volume of a 25 per cent w/v solution ofhydroxylamine hydrochloride and 3 volumes of 2 M sodium hydroxide.Add 2 ml of 2 M hydrochloric acid and 1 ml of ferric chloride solution and mixviolet-pink colour develops.
  34. 34. 2.U.V spectrophotometric method :Assay5/4/2013Yalamarty pharmacy college35Weigh accurately 20 capsules50mg equivalent of IndomethacinAdd 10 ml of water and allow to stand for 10 min,with occasional swirling.Add 75 ml of methanol, shake well,Add sufficient methanol to produce 100.0 ml and filter if necessary.To 5.0 ml of the filtrate add sufficient of a mixture of equal volumes of methanoland phosphate buffer pH 7.2 to produce 100.0 ml.Measure the absorbance of the resulting solution at the maximum at about 320 nmCalculate the content of indomethacin taking 193 as the specific absorbance at 320 nm.
  35. 35. 5/4/2013Yalamarty pharmacy college36•High Performance Thin Layer Chromatographic Analysis of Paracetamol andEtodolac in Combined Tablet Dosage Form.•Quantitative Analysis of Antipyretics and Analgesics in Solid Dosage Forms by PowderX.Ray -Diffraction.•Analytical method development and validation of Piroxicam by RP-HPLC.•Simultaneous estimation of nimesulide and paracetamol in marketed formulation by uv-spectroscopyRecent method of analysis
  36. 36. CONCLUSIONI here by conclude that there is a much necessityfor the study of analytical methods of Analgesicsand Antipyretics as they are widely used class ofdrugs…
  37. 37. REFERENCES• The Indian Pharmacopeia volume( ii) 2007Analgin page numbers : 117-118Aspirin page numbers: 127-128Aceclofenac page numbers: 62-63• Pharmaceutical Analysis Book: Takeru Higuchi. A.S.Doniger Kenneth A.Connors Antipyrine : (557-559), Amino pyrine: (559-561)• P. D. Sethi, “Quantitative Analysis of Drugs in Pharmaceutical Formulations”,.• B. Morelli, J. Pharm. Biomed. Anal.,1989, 7, 577.• http://analgesics and
  38. 38. THANKYOU