Spectrophotometric Determination Of Sodium Salicylate In .
MOJ Bioequivalence & BioavailabilityResearch ArticleOpen AccessSpectrophotometric determination of sodiumsalicylate in pharmaceutical preparations by couplingwith diazotized para–amino benzoic acidAbstractVolume 2 Issue 2 - 2016A rapid, sensitive and simple spectrophotometric procedure for the assay of thesmaller amounts measures from sodium salicylate at pharmaceutical preparations(topical–solution) was examined. The procedure is focus on a diazotization andreaction coupling between sodium salicylate and diazotized para–amino benzoic acidin alkaline medium for the formation of an intensive bright yellow soluble water colourwhich was being stable, which gives highly absorption at 452nm. The law of Beer wasIntroduced on the range of concentration from (2–30)μg.ml–1 of sodium salicylate, themolar absorptivity and the sensitivity of Sandell index were 8.5013 1031mol–1cm–1,0.0188μg/cm2 subsequently, The procedure does not need to the control of temperatureand the extraction by the solvent. The perfect circumstances for all colour increasingare portrayed and the examined procedure has been very good application on the assayof sodium salicylate at topical–solution preparations. The general excipients materialsand additives did not affect the examined procedure.Mohauman Mohammad AL–RufaieChemistry Department, Kufa University, IraqCorrespondence: Mohauman Mohammad AL–Rufaie, KufaUniversity, College of Science, Chemistry Department, Iraq,Email edu.iqReceived: July 17, 2016 Published: September 20, 2016Keywords: diazotization coupling reaction, spectrophotometric determination,sodium salicylate, para–amino benzoic acidIntroductionII. Heating–cooling water bath (Haake, Fe3).Sodium salicylate is the crystalline powder and white or almostwhite colour, or crystals with small, colourless or flakes shiny, waterfreely soluble, ethanol sparingly soluble (96per cent). It is a sodium2–hydroxybenzene carboxylate, C7H5NaO3, where as its chemicalstructure is1. Sodium salicylate was a salt for sodium with salicylicacid. It was formed by the reaction between sodium phenolate andcarbon dioxide by using higher pressure and temperature. In theliterature ,Where it had extracted by methyl salicylate that it wasobtaining from winter green plants or from sweet birch tree that resultfrom the bark by adding it with surplus of consented solution (sodiumhydroxide) and making reflux operation for it with heating.2 Thesubstance is utilized as therapy as an antipyretic and a pain relieving.Sodium salicylate additionally performs about as non–steroidalcalming (NSAID) drug, also it affects as anti cancer in the infectedcells3–5 and otherwise necrosis.6 It was using as Potential alternativefor aspirin drug that was giving to sensitive people for this drug.It may additionally be utilized as a phosphor for the discovery ofvacuum ultraviolet radiation and electrons.7 In the present work, thestable diazotized para–amino benzoic acid reagent has been proposedto determine sodium salicylate in pharmaceutical preparations(topical–solution) by the reaction (azo–coupling) in basic medium.The serious splendid yellow that was resulting in the product it wasspectrophotometrically computed at 452 nm. The new analyticalmethod is accurate, rapid and simple. The procedure was making avery good application in the investigation for sodium salicylate inpharmaceutical preparations (topical–solution).Experimental apparatusI. Every absorbance and spectral estimations were performed ondouble–beam applied UV–Visible 160 digital recording spectrometer (Japan).Submit Manuscript http://medcraveonline.comMOJ Bioequiv Availab. 2016;2(2):17‒21III. Analytical balance (Sartorius BL 210S).IV. pH meter, Jenway 3020.Material and reagentsThe Chemical substances that were utilized in the procedurewith very high purity degree and did not required to purification, allsolutions were obtained by the next steps.Sodium salicylate (500μg.ml–1) solutionThis solution is supplied by dissolution for (0.05g) of sodiumsalicylate (SDI) in (100) mL deionized water. This solution is at thatpoint exchanged to a dim bottle where it is steady for no less than 1month.1Para–amino benzoic acid (3x10–3M) (Diazotizedreagent solution)It was obtained by dissolution (0.01 gm) of para–amino benzoicacid (Fluka) with highly purity in (5mL) of deionized water afterthat (2mL) of 1 M HCl (BDH) was added and shacked well, thenContinued by adding of (0.009gm) from sodium nitrite (BDH) shakecompletely, after that the volume was diluted to (25mL) and the wascooling at temperature degree (5 C) for 30min, The solution wastaken to a dark bottle and leaved in the refrigerator that was steadyfor two weeks.Hydrochloric acid (BDH) (1M)It was provided by dissolution reasonable measure of concentratedhydrochloric to (100 mL) by deionised water.17 2016 AL–Rufaie. This is an open access article distributed under the terms of the Creative Commons Attribution License, whichpermits unrestricted use, distribution, and build upon your work non-commercially.
Copyright: 2016 AL–RufaieSpectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling withdiazotized para–amino benzoic acidSodium hydroxide (BDH) (0.5M)It was supplied by dissolution (2.0gm) of sodium hydroxide at(100mL) volumetric flask; the volume was completed to the lebal withdeionized water.ProcedureSeparately, volumetric flasks (25mL), the volumes was increasingof (500μg.ml–1 ) sodium salicylate from the standard working solutionwere exchanged to cover a range between (2–30)μg.ml–1 in the enddissolution, (0.5M) sodium hydroxide (1mL) solution, (2 mL) formdiazotized para–amino benzoic acid solution ( 0.003M) are added anddissolute to the lebal by deionized water. After that it was mixing verywell, then it was leaving for (15min) at (25 C), the intensive brightyellow colour for the result was gave the highly absorbance measuredat 452 nm against a blank reagent that was including all the materialswithout the sodium salicylate and the calibration curve was built.18away for (15minutes), the measured absorbance for this solution wasat 452nm. The salicylic acid concentration was given by utilizing thecalibration curve officially made and portrayed previously.This procedure was obtained for 3 trade kinds for topical–solutionthat was giving in the followingI. Avomack topical–solution (MECP.Riyadh–KSA): containing16.7% w/w Salicylic acid according to the product label.II. Duo film topical–solution (ITD, Sligo, Ireland): containing16.7% w/w Salicylic acid, according to the product label.III. NOCAL topical–solution (Jordan): containing 10% w/w Salicylic acid, as indicated by the item mark.Furthermore, the % Salicylic acid produced by the suggestedtechnique is as per the following.a. Every of the values that was utilizing in the table It was relateswith the quantity Every of the values that was utilizing in theTable*Assay procedure for salicylic acid in pharmaceuticalpreparations.b. Sodium salicylate, It was result from the multiply of the quantity of the salicylic acid per the sample by the conversion factorof 1.159, which was being equal to the output of dividing themolecular weight of sodium salicylate on the molecular weightof the salicylic acid.A topical–solution sample (25mL) was conveyed to volumetricflasks (100mL) then it was dissolute to the mark with deionized water.An aliquot for this solution (1mL) was put in volumetric flask (25mL),(2mL) (0.003M) diazonium agent, 1mL (0.5M NaOH), that wereadding , the completed volume to the lebal by deionized water, putTable 1 Salicylic acid investigation in some pharmaceuticals by utilizing the suggested techniquePharmaceutical productConc. salicylic acidµg. ml–1E%Rec. %RSD % n 5Conc. sod. salicylate µg. .329.867Duo 597Avomack Topical–solutionResults and discussionThe perfect reaction circumstance was studied, the impacts ofdifferent parameters on the optical characteristics for the azo colourhave been examined and the reaction circumstances are given.a. Reagent volume effectThe diazonium reagent (0.003M) volumes was examined byutilizing the range between (0.1–5 mL) on the absorbance intensity, itwas has been studying (2 mL) volume was the perfect volume.b. Acid volume effectThe presence of acid that was adding in the suggested procedureresulted in a increasing on the absorbance intensity for the formedproduct, so thus, acids like CH3COOH, HCl, H2SO4 and HNO3 arechecked up, all these acids was giving verging on equivalent intensity,therefore HCl was chosen for the next tests and, (2mL) volume wasthe perfect from the chosen acid that was obtaining highly sensitivewhich it utilized in following experiments.c. Base volume effectThe colour product formed was giving highly absorbance and itwas making more stable and intense in basic medium, so that, thevarious basic solutions effect on the colored result were examinedlike ammonium hydroxide sodium hydroxide, sodium acetate, sodiumcarbonate and potassium hydroxide. Highly stability and sensitivitywere given just when the reaction was performed with the attendanceof sodium hydroxide solution. The various concentrations of NaOHeffect were examined, (0.1–4M) volumes for the using base withconcentration (0.5M) appears to be ideal. The (0.5M) NaOH volumeseffect were as well examined between (0.1 to 5mL) (1mL) volumeswas the perfect volume and utilizing in the next tests.Citation: AL-Rufaie MM. Spectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling with diazotized para–aminobenzoic acid. MOJ Bioequiv Availab. 2016;2(2):17‒21. DOI: 10.15406/mojbb.2016.02.00020
Spectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling withdiazotized para–amino benzoic acidd. Order addition effectThe ideal order of addition that obtains the maximum absorptionwas (D B R) wherever (B base, D drug substance and R reagent)which was choosing in the following experiments.Copyright: 2016 AL–Rufaie190.0821 respectively. The beer’s law was given negative deviation atthe concentrations up to (30μg.ml–1) from the sodium salicylate. Themolar absorptivity was 8.5013 103l mol–1 cm–1.e. Temperature effectThe produced compound the studied procedure was examined atvarious temperatures. The absorbance values that obtained from Theoutcomes demonstrate that it was staying about consistent in the rangeof temperature 0–70 C, While, the absorbance value at the increasingtemperatures was Reduced, demonstrating the disintegration of theresult on the heating for a long time. The stability of the coloredcompound was between 15–20 C so that, this range of temperaturewas chosen in examined procedure.f. Reaction time effectThe highly intensity of colour arrived after that the sodiumsalicylate was reacting instantly with the solution of reagent. It wasmaking steady after time (15 minute). So that (15 minute) evolutiontime was taken as the prefect in the common method of assay. Thecolour resulted was steady for (2 days).The practical circumstances for the investigation for sodiumsalicylate were instituted. The reaction Diazonium happened in theacidic medium8 and (1M) concentration for hydrochloric acid waschosen,9 the absorbance for the colour compound formed has beenhighly stable and intense in basic medium.10Figure 2: The spectra of absorptionA: sodium salicylate (20μg.ml-1) Para-amino benzoic (3x10-3) (productcompound) versus the reagent (blank).B: The Blank reagent solution versus D.W.Absorption spectra11Precision and accuracy13The dilute solutions from sodium salicylate in under the foregoingfrom the Practical circumstances, was blending with diazotizedpara–amino benzoic acid in Attend the sodium hydroxide, the brightyellow intense colour compound instantly established. It gives highlyabsorption at 452nm at the same time the reagent solution (blank)gives no absorption at the same wavelength Figure 1 gives the spectraof absorption. The highly absorption wavelength was at 452nm it wasyet utilized for the next determinations.To investigate the precision and accuracy of the calibration curve,sodium salicylate was designating at three various concentrations.The results appeared in Table 2 was demonstrated a good satisfactoryaccuracy and precision.Product nature of and the mechanism of reaction14,15To observe the structure for the product compound (the ratiobetween sodium salicylate to diazotized para–amino benzoic acid) forthe intense bright yellow azo colour that was resulting from reaction,mole–ratio method and Job’s method of continuous variations havebeen utilized. The data that was resulting discover that the colour hasbeen established by the reaction of sodium salicylate with diazotizedpara–amino benzoic acid with a ratio of 1:1, Figure 3, Figure 4demonstrating a mono azo colour with possibly of the next schema.The stability constant was computed for the azo dye in the aqueoussolution, by using the circumstances of practical method, the constantwas equal to .28 106 1.mole–1. The regression equation was given, andthe analytical data for this method are obtained in the next (Table 2)Interferences effect16Figure 1 Chemical structure of sodium 2-hydroxybenzene carboxylateCalibration curve12By using the established practical circumstances. The linearrelationship between the concentration of sodium salicylate and theabsorbance was noted during the range of concentration (2–30μg.ml–1)(Figure 2) and a correlation coefficient and the intercept were 0.9990,The probably analytical enforcements were evaluated for the newsuggested Procedure, the interferences effect for the excipients on thedifferent levels for the quantitative assay of (20μg.ml–1)of Salicylicacid by utilizing the studied procedure have been tested, the resultsare obtained in Table 3.Application procedureThe examined procedure were checked up on the quantificationof salicylic acid in topical– solution preparations. Three kinds ofCitation: AL-Rufaie MM. Spectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling with diazotized para–aminobenzoic acid. MOJ Bioequiv Availab. 2016;2(2):17‒21. DOI: 10.15406/mojbb.2016.02.00020
Copyright: 2016 AL–RufaieSpectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling withdiazotized para–amino benzoic acidtopical–solution preparations having salicylic acid were tested, theywas obtaining a better precision and accuracy as appeared in Table 5.The examined procedure was given successful comparison with thestandard procedure.1Table 2 Precision and accuracy of examined procedureNo.Conc. of sodium salicylate mg per 25mlError %*Recovery*R.S.D 00.6870.99326.2260.769100.7691.2Table 3 Analytical properties of the developed method for the investigationof sodium salicylateParameterStudied methodRegression equationY 0.0531x–0.0821Linear range(μg ml )2–30–1Correlation coefficient, r0.999Detection limit0.0642(μg ml–1)Average of recovery %99.702Average of RSD %0.854Sandell’s sensitivity0.0188Figure 3 Calibration curve of sodium salicylate (ss)(μg cm–2)Molar absorptivity8.5013*103(l mol–1 cm–1)Table 4 Excipients effect on the investigation of (20μg.ml–1) of Salicylic acidExcipientConc. of Salicylicacid µg.ml–1E%REC% 51Starch19.8–199Mg 0.221.198.9Benzoic acid20.1250.625100.625manitol19.88–0.699.4Figure 4 Mole ratio plotTable 5 Application of the examined and standard procedures for theinvestigation of topical–solution having Salicylic acidPharmaceuticalpreparationRec.* % proposedmethodRec.* % standardmethodsodium salicylatePure99.702100.2Avomack Topical–solution99.28498Duofilm Topical–solution100.513102NOCAL Topical–solution100.51399.620Figure 5 Continuous variation plotCitation: AL-Rufaie MM. Spectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling with diazotized para–aminobenzoic acid. MOJ Bioequiv Availab. 2016;2(2):17‒21. DOI: 10.15406/mojbb.2016.02.00020
Spectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling withdiazotized para–amino benzoic acidCOOH NaNO2H2NHcooling212. Lehman JW. Operational Organic Chemistry. 4th ed. 2009. N2COOH3. Klampfer L, Jörg, Hans–Georg W, et al. Blood. PMID.1999;93(7):942386.4. Rae C, Susana L, Steven JT, David JM. Proceedings of the NationalAcademy of Sciences of the USA, 2007;104(31): 12790.COONa N2NaOHCOOHOHHOOCCopyright: 2016 AL–RufaieNNOHCOONa5. Stark LA, Kirsten R, Owen JS, et al. Aspirin activates the NF–κBsignalling pathway and induces apoptosis in intestinal neoplasia intwo in vivo models of human colorectal cancer. Carcinogenesis.2007;28(5):968–976.6. Schwenger P, Edward YS, Jan V. Inhibition of Tumor NecrosisFactor–induced p42/p44 Mitogen–Activated Protein Kinase Activation by Sodium Salicylate. The Journal of Biological Chemistry.1996;271(14):8089.7. Samson J. Pied Publications. 2012. 432 p.Figure 6 Colored Azo dye8. Morrison RT, Boyed RN. Organic Chemistry. 3rd ed. 1973. 451 p.Conclusion9. Al–Abachi MQ, Al–Delami AMS, Al–Najafi AS. Analyst.1988;113:1661.A sensitive, simple, rapid and precise spectrophotometricprocedure has been evaluation for the investigation of microgramquantities of sodium salicylate in the aqueous solution depended onthe diazotization reaction coupling with para–amino benzoic acid theprocedure does not need to the control of temperature control andsolvent extraction.AcknowledgementsNone.Conflict of interestThe author declares no conflict of interest.References1. British Pharmacopoeia. The Stationery Office on behalf of the Medicines and Healthcare products Regulatory Agency (MHRA). 5th ed.London, 2007.10. Roberts JD, Caserio MC, Benjamin WA. Basic Principles of OrganicChemistry. New York; 1964.11. Al–Rufaie MMW. Journal of pharmacy and pharmaceutical sciences.2016;5(3):172.12. Abdul Satar RS. Ph. D. Thesis, Baghdad University. Iraq; 2006.13. Al–Rufaie MM, Al–Sharefy AN, Kathem KH. SpectrophotometricDetermination of Doxycycline Hyclate in Pharmaceutical PreparationsUsing Oxidative coupling reaction. Journal of Applicable Chemistry.2013;2(4):931–939.14. Rathod KM, Thaker NS. Synthesis and Antimicrobial Activity of AzoCompounds Containing m–Cresol Moiety. Chemical Science Transactions. 2013;2(1):25–28.15. Marmion DM. Hand book of colorant. New York: Wiley; 1999.16. Al–Rufaie MM, Al–Sharefy AN, Kathem KH. International Journal ofUni. Pharmacy and Bio Sciences. 2013;2(4):2319.Citation: AL-Rufaie MM. Spectrophotometric determination of sodium salicylate in pharmaceutical preparations by coupling with diazotized para–aminobenzoic acid. MOJ Bioequiv Availab. 2016;2(2):17‒21. DOI: 10.15406/mojbb.2016.02.00020
Para–amino benzoic acid (3x10–3M) (Diazotized reagent solution) It was obtained by dissolution (0.01 gm) of para–amino benzoic acid (Fluka) with highly purity in (5mL) of deionized water after that (2mL) of 1 M HCl (BDH) was added and shacked well, then Continued by adding of (0.009gm) from sodium nitrite (BDH) shake
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