ANALYSIS OF ANALGESICS and ANTIPYRETICS

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Analgesics are a class of drugs used to relieve pain by selectively inhibiting the perception of the pain. An antipyretic is a type of medication that will reduce fever by lowering temperature from a raised state. They are available in the form of tablets,capsules,ointments,syrups and parentrals.CLASSIFICATION OF ANALGESICS AND ANTIPYRETICS: SALICYLATES

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10/3/2012 Yalamarty pharmacy college 1 Presented by… J.N.V. Indira Devi M.Pharmacy 1 st year Pharmaeutical analysis Yalamarty pharmacy college ANALYSIS OF ANALGESICS and ANTIPYRETICS

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10/3/2012 Yalamarty pharmacy college 2 INTRODUCTION CLASSIFICATION MECHANISM OF ACTION: Analgesics Antipyretics METHOD OF ANALYSIS CONCLUSION REFERENCES

ANALGESICS:

ANALGESICS 10/3/2012 Yalamarty pharmacy college 3 Analgesics are a class of drugs used to relieve pain by selectively inhibiting the perception of the pain. ANTIPYRETICS An antipyretic is a type of medication that will reduce fever by lowering temperature from a raised state. They are available in the form of tablets,capsules,ointments,syrups and parentrals .

CLASSIFICATION OF ANALGESICS AND ANTIPYRETICS:

CLASSIFICATION OF ANALGESICS AND ANTIPYRETICS 10/3/2012 Yalamarty pharmacy college 4 SALICYLATES Na.salicylate Benorilate: ARYL ALKANOIC ACID/ARYL ACETIC ACID DERIVATIVES Indomethacine sulindac PHENYL ACETIC ACID/ PHENYL PROPIONIC ACID DERIVATIVES Ibuprofen Diclofenac PYRAZOLONES/ PYRAZOLODIENES: Antipyrin .Aminopyrine

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10/3/2012 Yalamarty pharmacy college 5 PARA AMINO PHENOL DERIVATIVES 1.Paracetamol, 2.Acetophenetidin QUINOLINE DERIVATIVES Ex:1.Cinchophen, , 2.NeoCinchophen N-ARYL ANTHRANILIC ACID/FENAMATES Ex: Mefenamic acid , Flufenamicacid OXICAMS/ENOLIC ACIDS Ex:Pyroxicam, Isooxicam SELECTIVE COX2 INHIBITORS: Ex: Etoricoxib Rofecoxib GOLD COMPOUNDS: EX: Aurothioglucose, aurofin

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10/3/2012 Yalamarty pharmacy college 6 OTHER ANALGESICS Opioids Alpha–2 agonists Thiazine derivatives Local Analgesics Morphine Oxymorphone Meperidine ( demerol ) Methadone Xylazine Meditomidine ( domitor ) Lidocaine ( xylocaine ) Benzocaine

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NSAIDs Prostaglandins pGE2 pGF2 Nerve ending of pain Pain Bradykinin histamine factors + Analgesic Mechanism block prostaglandins production Site of action: peripheral tissue ANALGESIC MECHANISM 10/3/2012 Yalamarty pharmacy college 7

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NSAIDs Pyrogen Prostaglandins pGE2 thermoregulatory center heat production ↑ Heat dissipation ↓ set point ↑ Fever Antipyretic Mechanism Block prostaglandins production Site of action CentralNervousSystem ANTIPYRETIC MECHANISM 10/3/2012 Yalamarty pharmacy college 8

METHOD OF ANALYSIS:

METHOD OF ANALYSIS 10/3/2012 Yalamarty pharmacy college 9 Aspirin Diclofenac sodium Aceclofenac Ibuprofen Paracetamol Analgin Antipyrine Indomethacine Mefenamic acid

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Aspirin 1.Titrimetric analysis : Assay method 2.Chromatographic method 3.Spectrophometric method Method of analysis Tablet Limits : 95.0 -105.0 % of the stated amount of Aspirin Uses: -Analgesic and antipyretic. -Anti rhemuatic . -Anti gout. -Anti platelet agent . Aspirin is 2-acetoxybenzoic acid.

Titrimetric analysis Assay of aspirin:

Titrimetric analysis Assay of aspirin . Equivalent factor:1ml of 0.5M HCl ≡ 0.04504g of aspirin Amount of aspirin=(B.R-S.R) * volume of NaOH added *(Actual molarity of HCl ) * E.F B.R Theoritical molarity of HCl

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2.Chromatographic Method of Analysis High 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 solvent with 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 in a volumetric flask and injected in to HPLC.

3.Spectrophometric Analysis visible Spectrophotometric method:

3.Spectrophometric Analysis visible Spectrophotometric method . .

Diclofenac sodium:

Diclofenac sodium Tablet Limits : 95%-105% of the stated amount of ibuprofen Method of analysis 1.U.V Spectrophotometric method 2.Potentiometric method Also known as Voltaren Sodium It ranks Second in sales (1983) world wide IUPAC name:2-{2-[(2,6-dichlorophenyl)amino]phenyl}acetic acid Uses: -Analgesic and antipyretic. -In rheumatic fever.

Assay of diclofenac sodium:

Assay of diclofenac sodium . 1.U.V spectrophotometric method Reference solution : A 1 % w/v solution of diclofenac sodium RS in methanol Calculate the content from the absorbance obtained.

2.Potentiometric method by Non-aqueous titrimetry:

2.Potentiometric method by Non-aqueous titrimetry 16 End point determined potentiometrically by plotting ∆pH/∆v on y-axis and volume of titrant added on x-axis. Equivalent factor:1ml of 0.1M HClO 4 ≡0.03181g of diclofenac sodium Amount of drug = volume of titrant consumed * Actual molarity of HClO 4 * E.F Theoritical molarity of HClO 4 0.2gm powder equivalent of diclofenac tablets+50ml glacial acetic acid Titrate against 0.1M HCl0 4

Aceclofenac :

Aceclofenac 10/3/2012 Yalamarty pharmacy college 17 IUPAC Name:[(2,6-dichlorophenyl)amino] phenylacetoxyacetic acid. Tablet Limits : 99%-110% of the stated amount of Aceclofenac Uses: -Analgesic and antipyretic. -In rhemuatoid arhritis .

Method of analysis: Titrimetric method::

Method of analysis: Titrimetric method: 10/3/2012 Yalamarty pharmacy college 18 Blank is performed. End point is determined potentiometrically by plotting ∆pH/∆v on y-axis and volume of 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.F Theoritical molarity of NaOH

Ibuprofen:

Ibuprofen Tablet Limits : 95%-105% of the stated amount of ibuprofen Method of analysis 1.Titrimetric method 2.U.V spectrophotometry IUPAC name: 2-[4-(2-methylpropyl)phenyl]propanoic acid Uses: -Analgesic and antipyretic. -In rhemuatoid arhritis . -In spondilitis .

1.Titrimetric method Assay of ibuprofen:

1.Titrimetric method Assay of ibuprofen . Equivalent factor:1ml of 0.1N NaoH≡0.02063g of ibuprofen. Amount of ibuprofen=vol. of NaOH consumed * Actual normality * E.F Theoritical normality 2.U.V spectrophotometric method Solvent: Chloroform Wave length:264 nm So, Ibuprofen present in bulk samples can be estimated

Paracetamol:

Paracetamol Method of analysis: Thin layer chromatographic method Colorimetric method Polarographic method IUPAC name: N-(4-hydroxyphenyl) acetamide Uses: -Analgesic and antipyretic.

1.Thin layer chromatographic method:

1.Thin layer chromatographic method Stationary Phase: l- Octanol, liquid paraffin Mobile phase: Acetone:water (1:9) Procedure : Semi-quantitative procedures relying on the visual comparison of sample spot size and Intensity with standards the acetaminophen is acid to p-aminophenol which is then separated (lO-lOOµg. /spot) by thin layer chromatography on a Silica Gel G layer. The p-aminophenol is eluted with 0.5N sodium hydroxide solution and determined spectrophotometrically at 240 nm .

2. Colorimetric method: a)With 2,4-DNB:

Reagents:1%w/v 2,4-dinitrobenzaldehyde in 5 % v/v 0.1N H₂SO 4 ,1N HCl The schiff’s base measured at 435nm 2. Colorimetric method: a) With 2,4-DNB Yellow colour

b)Diazotization with NED: :

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 HCL Procedure: b)Diazotization with NED:

3. voltammetric method: :

3 . voltammetric method: The peak current from acetaminophen in 0.10 M phosphate buffer pH 7.0 ( 41.30 ml of 0.10M Potassium dihydrogen phosphate into 58.70 ml of 0.10M disodium hydrogen phosphate) was measured with a glassy carbon electrode versus Ag/ AgCl . General Procedure A 20.00 ml of 30 μg ml -1 acetaminophen standard solution in 0.10 mol L -1 phosphate buffer pH 7.0 was pipetted into the voltammetric cell The cyclic voltammograms were obtained by scanning the potentials from -0.3 to +1.5 V vs. Ag/ AgCl at step potential of 0.0005 V and scan rate of 0.10 V/s.

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27 A direct calibration curve and the standard addition method were both used to evaluate the content of acetaminophen in commercial samples of paracetamol For the standard addition method, 20.00 ml of unknown sample solution in 0.1 mol L -1 phosphate buffer pH 7.0 was pipetted into the voltammetric cell. Five voltammograms were recorded after adding of 0.00, 0.50, 1.00, 1.50 and 2.00 ml of 1,000 μg ml -1 acetaminophen standard solution Procedure for paracetamol tablet samples

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10/3/2012 Yalamarty pharmacy college 28 Thin Layer Chromatography Method for the Determination of Paracetamol and Ibuprofen in Pharmaceutical Formulation The purpose of this study to obtain an efficient solvent for extracting paracetamol and ibuprofen from sample and a good eluent for separation between paracetamol and ibuprofen on the TLC plate. Adsorbant:silica gel 60 F 254 . Mobile phase:Ethylacetate : n-hexane, (75 : 25 v/v) Retardation factor ( Rf ) : Paracetamol : 0.24 Ibuprofen: 0.64 Resolution factor between paracetamol and ibuprofen was 6.4. The analyte spots were quantified using densitometry method : Paracetamol:244 nm Ibuprofen:260nm

Analgin :

Methods of analysis 1 . Iodimetry method 2. Colorimetry method 1. Iodimetry method: 1ml of 0.05 M iodine is equivalent to 0.01667 g of Analgin Analgin

2. Colorimetry method: :

Reagents:0.5M Phthalate Buffer: pH:4.0 0.5%w/v 1,2-napthaquinone-4-sulfanic acid (NQS)-sodium Procedure: 2ml of sample add 5ml of buffer + 1ml of NQS-sodium heat on water bath for 60°c for 40min extract with chloroform orange colour appears absorbance measured at 475nm. 2. Colorimetry method:

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METHOD OF ANALYSIS: 1.Gravimetric method 2.Colorimetric methods 3.Polarographic method IUPAC Name:1,5-dimethyl-2-phenyl-2,3-dihydro-1H- pyrazol-3-one Antipyrine Uses: -An analgesic and antipyretic that has been given by mouth and as ear drops. -Used in testing the effects of other drugs or diseases on drug-metabolizing enzymes in the liver.

1. Gravimetric method:

1. Gravimetric method The precipitate is weighed to determine the weight of antipyrine present.

2.Colorimetric method :

REAGENT SOLUTION: P-di methyl amino benzaldehyde (0.5g) is dissolved in a mixture of 4.5ml of concentrated sulphuric acid and 8.5ml of water. 2.Colorimetric method PDAB YELLOW COLOURED COMPLEX ANTIPYRINE Absorbance measured at 450nm.

3. Polarographic method :

Antipyrine is nitrosated to give a compound which is reducible at the dropping mercury electrode. Procedure: 3. Polarographic method

Mefenamic acid:

Mefenamic acid Assay: HPLC IUPAC Name: 2-[(2,3-dimethylphenyl)amino] benzoic acid Chromatographic system Column : Stainless steel 25 cm x 4.6 mm packed with octadecylsilane chemically bonded to porous silica. Mobile phase : Acetonitrile : ammonium phosphate: tetrahydrofuran (53:40:7) Flow rate : 1 ml/min Spectrophotometer : 254 nm Injection volume : 20 μl

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Test solution: Weigh 20 capsules 50 mg of Mefenamic acid 250 ml volumetric flask Add 5 ml of tetrahydrofuran Shake for 10 minutes with the aid of ultrasound Dilute with mobile phase & filter Reference solution: A solution containing 0.02 % w/v of mefenamic acid RS in the mobile phase. Inject alternately the test and the reference solution. Calculate the content of C 15 H 15 NO 2 in the capsules .

Indomethacin:

Indomethacin IUPAC Name 2-{1-[(4-chlorophenyl)carbonyl]-5-methoxy-2-methyl-1H-indol-3-yl}acetic acid Assay: Thin layer chromatography Test solution : Shake a quantity of the contents of the capsules containing 0.1 g of Indomethacin with 5 ml of chloroform filter and use the filtrate. Dilute 1 volume of the test solution to 200 volumes with chloroform. Mobile phase : A mixture of 70 vol of ether and 30 vol of light petroleum . PROCEDURE: Apply to the plate 10 μl of each solution. After development, dry the plate in air and examine in ultraviolet light at 254 nm.

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10/3/2012 Yalamarty pharmacy college 38 H igh Performance Thin Layer Chromatographic Analysis of Paracetamol and Etodolac in Combined Tablet Dosage Form. Quantitative Analysis of Antipyretics and Analgesics in Solid Dosage Forms by Powder X.Ray Diffraction. Analytical method development and validation of Piroxicam by RP-HPLC. Simultaneous estimation of nimesulide and paracetamol in marketed formulation by uv - spectroscopy Recent method of analysis

CONCLUSION:

CONCLUSION I here by conclude that there is a much necessity for the study of analytical methods of Analgesics and Antipyretics as they are widely used class of drugs…

REFERENCES:

REFERENCES The Indian Pharmacopeia volume( ii) 2007 Analgin page numbers : 117-118 Aspirin page numbers: 127-128 Aceclofenac 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 antipyretics.cwru.edu/ encycl /.com

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