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Spectrophotometric analysis of Drugs

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Spectrophotometric Research PPT

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Spectrophotometric analysis of Drugs

  1. 1. G.Sasikala & G.Venkateshwarlu* Dept. Of Chemistry , Osmania University , Hyderabad Quantitative Determination of Promethazine Hydrochloride & Prasugrel Hydrochloride By using FC Reagent : A Spectrophotometric Study
  2. 2. Promethazine Hydrochloride Promethazine hydrochloride[-meth′əzēn] a phenothiazine antiemetic, antihistamine, and sedative. Indications It is prescribed in the treatment of motion sickness, nausea, rhinitis, itching, an d skin rash and as anadjunct to anesthesia and pain control.
  3. 3. Prasugrel Hydrochloride Prasugrel is a member of the thienopyridine class of ADP receptor inhibitors, like ticlopidine (trade name Ticlid) and clopidogrel (trade name Plavix). These agents reduce the aggregation ("clumping") of platelets by irreversibly binding to P2Y12 receptors. Compared to clopidogrel, prasugrel inhibits adenosine diphosphate–induced platelet aggregation more rapidly, more consistently, and to a greater extent than do standard and higher doses of clopidogrel in healthy volunteers and in patients with coronary artery disease, including those undergoing PCI.
  4. 4. Folin–Ciocalteu Reagent • The Folin–Ciocalteu reagent (FCR) or Folin's phenol reagent or Folin–Denis reagent, also called the Gallic Acid Equivalence method (GAE), is a mixture of phosphomolybdate and phosphotungstate used for the colorimetric in vitro assay of phenolic and polyphenolic antioxidants. It is named after Otto Folin, Vintilă Ciocâlteu, and Willey Glover Denis.
  5. 5. Promethazine Hydrochloride • Because of the physiological significance the drug has been analysed by various methods like: 1. FIA Method- Flow Injection analysis Method 2. Electrophoresis Method 3. Potentiometric Method 4. Oxidative Coupling with sulphonilic acid 5. Titrimetric Method 6. By forming Choloroform extractable complexes with (BCG) Bromocresol Green 7. UV Visible Spectrophotometric Method
  6. 6. Prasugrel Hydrochloride • Because of the physiological significance the drug has been analysed by various methods like: 1. Visible Spectrophotometric Method 2. By forming Ion Pair complex with Bromo Phenol Blue ( BPB) 3. UV Visible Spectrophotometric Method 4. High Performance Liquid Chromatography Method ( HPLC) 5. Liquid Chromatography Method (LC) 6. Reverse Phase Liquid Chromatography Method (RP-LC) 7. Titrimetric Method – Based on the Oxidation of Drug by meta Venadate in acidic medium or Cerium(IV)Sulphate.
  7. 7. Analysis • Thorough Survey of Literature revealed that Folin–Ciocalteu reagent (FCR) is a sensative , Precise , accurate reagent for the analysis of Phenolic Materials • As the Above Mentioned drugs possess Phenolic Nature , the author is prompted to use this method for the above drugs for their analysis and validation. • The reagent does not only measure phenols, and will react with any reducing substance.
  8. 8. Experiment : Methods & Materials • A Double Beam systronics spectrophotometer 117 had been used along with An ELICO UV double beam spectrophotometer SL210 to record the spectra of the drugs, reagent and the product formed due to the interaction of the drug with the reagent was recorded.
  9. 9. Experiment : Materials • Drugs were procured from M/s. Harika Drugs Pvt Ltd , Hyderabad as Gift Samples . • Folin–Ciocalteu reagent (FCR) was supplied by Finar Chemicals (AR) grade , this was used without further Purification. • NaOH was supplied by SD fine Chem (AR) grade • Triple Distilled water was used for preparing Solutions.
  10. 10. Experiment : Materials Systronic Spectrophotometer Elico Spectrophotometer Quivites
  11. 11. Construction of Calibration • A stock solution of 1000μg/ml was prepared and diluted to a concentration range of 10 μg/ml to 80 μg/ml , to each solution 1 ml of the Folin–Ciocalteu reagent (FCR) , 1ml of NaOH was added and made up to the mark of 10ml using triple distilled water.
  12. 12. Experiment • The Experiment was repeated atleast for 6 times to get precise and accurate optical densities • Average 95% , 110% points falling within the range were taken.
  13. 13. Optimization of the factors effecting Absorbance: • Promethazine Hydrochloride produced blue colour with λ max 741 nm immediately after mixing the solutions . The intensity did not change even after 1 hr observation. • Prasugrel Hydrochloride too produced blue colur at λ max 963 nm after heating the contents for 50 minutes on a water bath at 60°Celsius , further increase in time and temperature did not show any effect.
  14. 14. Optimization of the factors effecting Absorbance: • Effect of NaOH : The concentration of NaOH was varied between 0.1 M to 1 M optimum absorbance was found at 0.5M solution. • Effect of Concentration of the Reagent: To test the Reagent Concentration 5ml of the drug was uniformly taken into 6 standard flasks and 1% to 6% of the reagent was added . It was observed that the concentration of the reagent dint effect the OD appreciably
  15. 15. Validation • The methods developed have been validated in terms of LOD, LOQ, limits of Beers law, Robustness, Druggedness, Accuracy & Precision are presented in the table.
  16. 16. Table Name of the Property Promethazine HCL Prasugrel HCL λmax 741 nm 963 nm Beer’s law limits (µg/ml) 10-80 10-80 Sandell’s sensitivity (µg/Cm²) 0.0793 0.0854 Std. Dev. of intercepts 0.002723 0.002066 LOD (µg/ml) 0.713 0.582 LOQ (µg/ml) 2.139 1.746 Slope ,b 0.0126 0.0117 Intercept, a 0.06852 0.09028 Correlation coefficient 0.9469 0.9973 Regression equation 0.0685+ 0.0902+ Y=a+bX* ( X= Conc. Of Drug) 0.0126X 0.0117X
  17. 17. Application of the Methods for the Analysis of Pharmaceuticals • Promethazine HydroChloride name : Phenergan Injection 4 voils of 25 mg/2ml ABBOTT company were purchased . • Solutions were combined and diluted to the required concentrations of working range.Recovery studies have been performed to determine accuracy and precision of the method.
  18. 18. Application of the Methods for the Analysis of Pharmaceuticals • Prasugrel Hydrochloride : Dry 10mg tablet of this drug with brand name : Prasusafe manufactured by MSN laboratories was ground well into a motor & pestle. • Powder Equivalent to 25mg of the drug was dissolved in 100ml of triple distilled water , filtered with 41 micron Watt paper and the solutions was diluted to the concentration of working range.
  19. 19. Application of the Methods for the Analysis of Pharmaceuticals • Precision and accuracy are determined in terms of %RSD and the reproducibility by performing 5 replicates. • The applicability of methods are statistically analysed by performing t-test and F-test with a standard method available in literature.
  20. 20. Table : Parameters Using Pure Sample Name of the Drug Taken OD Found OD % Recov ery RSD% t-test F- test Promethazine Hydrochloride 0.952 0.875 0.738 0.640 0.961 0.876 0.733 0.643 100.94 100.11 99.32 100.46 0.808 1.425 3.429 Prasugrel Hydrochloride 1.016 0.896 0.774 0.670 1.021 0.906 0.776 0.675 100.49 101.11 100.25 100.74 0.365 0.6094 2.057
  21. 21. Conclusion • The Methods Developed are useful for the analysis of the drugs either in Bulk Industries or in Pharmaceuticals.
  22. 22. Acknowledgement • The authors are thankful to the Head , Department of Chemistry , Osmania University , Hyderabad -500007, for providing facilities. • Special Thanks to the Chairman & Principal of Princeton PG College , Ramanthapur , Hyderabad for their Support.
  23. 23. References • 1. S.M. Su1tan,Y.A.M. Hassan, and A.M. Abukibash,chemiluminescence assay of promethazine hydrochloride using acidic permanganate employing flow injection mode operated with syringe and peristaltic pumps,Talanta,Vol.59,(2003),pp1073-1080. • 2. R.l.Baxter,G.Sveh1a,B.Kem and A.D.Woolfson, Determinationof promethazine by anodic differential poise voltammtery, Anal.Chim.Acta,Vol.164,(1984),pp171-181. • 3. Ni YongnianLi Wang, and skokot, Voltammetric determination of chlorpromazine hydrochloride and promethazine hydrochloride with the use of multivariate calibration, analchim Acta, Vo1.439,(2001),pp159-168. • 4. G.-Taylor and J.B.Houston, Simultaneous determination of promenading and two of its circulating metabolites by high performance liquid chromatography,l.chromatogr.B,V01.230,(1982),pp194-198. • 5. P.G.H.M. Muijselaar,H.A. Claessens and C.A. Crnmers,Determination of structurally related phenothiazines by capillary zone electrophoresis and micellar electrokinetic chromatography, J.Chromatogr.A,Vo1.735, (1996), pp395- 402. • 6. F.J.Lara, A.M. Garcia- Campana F.A1es- Barrero and J.M.bosquesendea, Anal.chim.Acta, Determination of thiazinamium, promazine and promethazine in pharmaceutical formulations using a CZE method, Vo1.535,(2005),pp101-108. • 7. J.M. Calatayud, S.N. Sarrion, A.S. Snmpedro, and C.G. Benito,Determination of promrthazine hydrochloride with bromophenol blue by a turbidimetric method and flow injection analysis, Microchem. J.,Vo1.45,(1992),pp129-136. • 8. S.M.Golabi, and M.showkati-shishevan, potentiometric titration of phenothiazine compounds in chloroform and its use.in pharmaceutical analysis, Talanta,vol. 38,(1991), pp1253-' 1256. • 9. A.S.1ssa, and M.S. Mahrous, Titrimetric determination of some phenothiazine derivatives, with ferricyanide, Talanta,V01.31,41984),pp287-288. • 10. E.A.lbrahim, A.S. Issa, M.A. Abdel salad, and M.s.Maitrous, The ues of chloranil for spectrophotometric determination of some tvanquillizers and antidepressants, Talanta, V01.30,(1983),pp531-533. • 11. K.Basavaiah, Determination of some psychotrop phenothiazine drugs by charge-transfer complication reaction with chloranilic acid, IlF|armaco, Vo1.59,(2004),pp315-321. • 12. E.Regulska,M. Tarasiewicz, and H.puzanowska TarasiewiczExtractive-spectrophotometric determination of some
  24. 24. References • 13.Baker W L, White C M; Role of Prasugrel, A Novel P2Y12 Receptor Antagonist, in the Management of Acute Coronary Syndromes. American Journal of Cardiovascular Drugs Aug 1, 2009; 9 (4): 213-229. • 14. Wiviott S D, Braunwald E, McCabe C H et al. "Prasugrel versus clopidogrel in patients with acute coronary syndromes". N Engl J Med 2007; 357 (20): 2001–15. • 15. "FDA Drug Safety Communication: Reduced effectiveness of Plavix (clopidogrel) in patients who are poor metabolizers of the drug". Drug Safety and Availability. Food and Drug Administration (United States). March 12, 2010. • 16. Angiolillo D J, Saucedo J F, DeRaad R et al. Increased platelet inhibition after switching from maintenance clopidogrel to prasugrel in patients with acute coronary syndromes. J Am Coll Cardiol. 2010; 56: 1017-23. • 17. O'Riordan, Michael. "Switching from clopidogrel to prasugrel further reduces platelet function".http://www.theheart.org. • 18. Tian E R, Ruterbories K J; Verburg E M; Weerakkody GJ, Kurihara F N, American Society for Pharmacology and Experimental Therapeutics. 2007; 35(6):917-921. • 19. Farid N A, McIntosh M, Garofolo F, Wong E, Shwajch A, Kennedy M, Young M, Sarkar P, Kawabata K, Takahashi M, Pang H; Rapid Communications in Mass Spectrometry. 2007; 21(2):169-179. • 20. Borole T C, Mehendre R, Damle M C, Bothara K G; Development and validation of stability indicating HPTLC method for determination of Prasugrel. J Chem Pharm Res. 2010; 2(4):907-913]
  25. 25. Thank You

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