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IDENTIFICATION & QUANTITATIVE DETERMINATION OF PRESERVATIVES IN PHARMACEUTICALS BY T.PRAVALLIKA 11031S0406 M.PHARMACY (P.A & Q.A)

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Preservative is a chemical substance that used to prolong the shelf life of pharmaceutical product

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Why addition of preservatives is needed in pharmaceutical preparations ? The pharmaceutical products especially those containing high water content are prone to alteration and degradation by micro organism during storage

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Preservatives are two types Anti microbial Anti oxidants

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TYPES OF ANTI MICROBIAL PRESERVATIVES Anti-fungal : Parabens : methyl paraben , propyl paraben Acids & their salts : benzoic acid, sod.benzoate , sorbic acid, sod.sorbate Anti- bacterial : Quarternary ammo. comp: cetrimide , benzalkonium.cl Mercurials : phenyl mercuric nitrate, thiomersal

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Alcohols: benzyl alcohol, phenyl ethyl alcohol Phenols: phenol, cresol, 4-chloro-3-methyl phenol Biguanides : chlorhexidine

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TYPES OF ANTI OXIDANT PRESERVATIVES Phenolic : BHA, BHT, TBHQ, gallic acid, propyl gallate , tocopherol ( vit E) Reducing agents: ASA, TGA, ASP Sulphites : sod.sulphite , sod bisulphite , sod.metabisulphite , thio glycerol Synergistics & chelating agents: EDTA, lecithins

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QUANTITATIVE DETERMINATION OF ANTI-MICROBIAL PRESERVATIVES High Performance Liquid Chromatographic methods Gas Chromatographic method Thin Layer Chromatographic Capillary electrophoresis

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Flow injection analysis Spectrophotometric methods Titrimetric methods Electrochemical metho ds

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CAIPLLARY ELECTROPHORESIS : can be used to separate ionic species by their charge and frictional forces and hydrodynamic radius i.e.  based on their size to charge ratio in the interior of a small capillary filled with an electrolyte FIA: is an automated method in which a sample is injected into a continuous flow of a carrier solution that mixes with other continuously flowing solutions before reaching a detector .

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PARABENS HPLC GC TLC FIA SPECTROPHOTOMETRY CAPILLARY ELECTROPHORESIS METHOD ACIDS & SALTS HPLC TLC SPECTROPHOTOMETRY ELECTROCHEMICAL METHODS CAPILLARY ELECTROPHORESIS METHOD QUARETENARY AMMONIUMCOMPS CAPILLARY ELECTROPHORESIS METHOD HPLC GC TLC FIA SPECTROPHOTOMETRY TITRIMETRY

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MERCURIALS COMPS HPLC SPECTROPHOTMETRY ELECTROCHEMICAL METHOD TITRIMETRIC METHODS ALCOHOLS HPLC GC SPECTROPHOTOMETRY ELECTROCHEMICAL METHOD PHENOLIC COMPS HPLC GC FIA SPECTROPHOTOMETRY ELECTROCHEMICAL METHOD

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PARABENS HPLC : -Regular or silanol -deactivated C18 or C8 columns with UV detection are the most common configuration for the analysis of parabens . For parabens in liquid pharmacueticals Mobile phase: mixture of methanol-and phosphate buffer of pH 7.05. Detection :254 nm. For semi solid dosage forms RP-HPLC , mobile phase: mixture of methanol- acetonitrile -water. Detection :238nm. For solid dosage forms RP-HPLC, mob.phase : acetonitrile with phosohate buffer at pH-7 detection :276 nm. For parabens in pediatrics RP-HPLC with C8 column and a mobile phase of pH-4 used detected at 260nm.

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Electrokinetic capillary electrophoresis (CE) was reported for the determination of methyl, ethyl, propyl and butyl parabens using fused silica capillary column and applied voltages of 22, 25, 27 and 30 kV respectively. The UV detection was carried out at 220 nm. Method: by use of run buffer containing 20 mM borate buffer (pH 9.0) with 10% methanol and by applying voltage of 20 kV, a low hydrodynamic injection of 10 s, and detecting the signals at 200 nm. Moxifloxazin was used as an internal standard. All parabens were separated within 10 min. FIA: flow injection– chemiluminescence (FIA-CL):The method is based on the fact that parabens greatly enhance the chemiluminescence reaction between the cerium (iv)- rhodamine system in strong sulphuric acid. The method has very low detection limits and wide dynamic range.

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GC: Extraction of parabens derivatization by reaction with hexamethyldisilazane and heptafluorobutyric anhydride determination of parabens using FID TLC: Ointments – mobile phase :n-pentane-glacial acetic acid mixture Detection: densitometry measurement at 260 nm suspension were determined by RP-TLC plates. Detection :densitometry measurement at 254 nm Spectrophotometric methods: acidic extract of paraben add methanol and NaOH sol measuremant at 240-330nm

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ACIDS AND THEIR SALTS: Capillary electrophoresis methods: Method similar to parabens Micellar Electrokinetic chromatography and microemulsion electrokinetic chromatography were used for the determination of benzoic acid, sorbic and parabens in pharmaceutical products. HPLC: RP-HPLC with C8 column using an UV detector at 247 nm method was for the determination of benzoicacid . solid phase extraction and HPLC method for the simultaneous determination of dehydroacetic acid, benzoic acid, sorbic acid and salicylic acid in cosmetics, using tetra-n-butyl ammonium hydroxide as an ion pair reagent. Sorbic acid was determined by RP-HPLC with C18 column Ion chromatographic technique was also applied for the analysis of these acids in pharmaceutical products.

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TLC: Determination of benzoic acid , sorbic acid in bulk powder and formulation using Different, developing solvents and U.V detection at 254nm Spectrophotometric methods : Determined directly by UV spectrophotometry at 256nm in o.1M HCl . Where as sorbic acid in syrups determined at 250nm. QUARTERNARY AMMONIUM COMPS: Capillary electrophoresis: Used for determination of bkc , separated at potential of 15kv detected at 200nm Cetyl pyridinium chloride determined with uv detection or HPLC with conductometric detection HPLC: BKC- cyano column and mobile phase – aq acetonitrile at pH-5 detected at 262nm Bkcs can also deremined by RP-HPLC with water – acetonitrile mixture as mob phase, at 210nm

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GC: Bkc + pot.t-butoxide Pyrolysis Ter -amine of bkc Extracted into benzene Extract analysed on SE-30 column Pyrolused prdct identified by GC-MS TLC: The chain homologues of BKCs, cetrimide , CPB and CPC were separated on TLC and detected by the yellowish-brown spots on a colorless background. They were quantified by UV densitometry. FIA: The determination of BKCs after the reaction with quinine - bromophenol blue present in the carrier stream, followed by on-line extraction and measurement at 610 nm BZC was determined by FIA where the sample was injected in stream containing quinidine and bromochlorophenol blue in 1,2-dichloroethane. The product in the organic layer was measured at 605 nm thiomersal and BKCs in the simultaneous determination determined by FIA with photometric detector.

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SECTROPHOTOMETRIC METHODS: Preservatives including cetyltrimethyl ammonium bromide, CPB, and dimethyldodecylbenzyl ammonium bromide react with 1-(4-nitrophenyl)-3-(4-phenylazophenyl) triazene and the produced colors are measured at 530, 540 and 590 nm, respectively A colorimetric method for the determination of BKC in eye-drops based on ion-pair formation between BKC and eosin.  The method is based on measurement of the decrease in absorbance of eosin TITRIMETRIC METHODS: BZC ,CPC, acronil determined by titration with sod.tetraphenylborate or sod.dodecyl sulfate and the end point was detected by potentiometer or tetrabromophenol-phthalein ethyl ester as indicator.

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MERCURIALS HPLC: Spectrometric methods: A spectrophotometeric method for the determination of phenylmercuric nitrate based on the formation of a ternary complex between Hg (II) (produced after digestion by HCl -HNO 3 ) with 4-(2-pyridylazo) resorcinol and benzyl- hexadecyldimethyl ammonium chloride in phosphate buffer of pH 7.2. The reaction product was extracted into CHCl 3 and measured at 525 nm.

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Electro chemical methods: Polarographic and amperometric methods are used for determination of mercurials Titrimetric methods: PMN up on titration with KI end point detected by iodode -iodide selective electrode ALCOHOLS: HPLC: Benzyl alcohol and its oxidative product, benzaldehyde , were determined in parentral solutions by RP-HPLC using C8 column and UV detection at 240 nm GC: Gc with FID is used for dtermination of chlorbutanol , benzyl alchohol , Spectrophotometric methods: amperometric enzyme electrode – response measured at +0.7V v/s SCE Polarigraphic technique is also used

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PHENOLS: HPLC: RP-HPLC method coupled with C18 column and UV detection at 271nm reported for phenol, cresol using nicotinic acid as internal std HPLC with fluorescence detector for determination of chlorocresol , chloroxylenol GC: Gc with FID for phenol determination The method is based on the derivatization of phenols with pentafluoropyridine , followed by adsorption of the derivatives on anion-exchange solid phase cartridge The derivatives were determined by GC-MS. A capillary GC method was developed for the simultaneous analysis of camphor and m- cresol in commercial cream products

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FIA: FIA with quinine sensitized photo- oxidation technique with quenched luminal chemiluminiscence (CL) detector. reverse prevaporation FI method coupled with on-line derivatisation and amperometric detection at +0.62 V versus Ag/ AgCl , was developed for the determination of trace phenol in aqueous solution SPECTROPHOTOMETRIC METHODS: Phenol in ear drops was determined by direct measurements of the absorbance in NaOH solution at 288 nm. Phenol and salicylic acid in formulations were determined after azo - dye formation with diazotized sulphanilic acid as a reagent ELECTROCHEMICAL METHOD: an amperometric sensor for the determination of phenolic compounds using a glassy carbon electrode doped with copper dipyridyl complex as biomimetic catalyst and measurements were carried out versus SCE.

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REFERNCES 6. W. J. Reilly, "Pharmaceutical Necessities", in: "Remington: The Science and Practice of Pharmacy",

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