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PROJECT TOPIC- NSPECTROPHOTOMETRIC DETERMINATION OF RISPERIDONE AND MOXIFLOXACINBY CHARGE TRANSFER COMPLEXATION USING CHLORANILIC ACID

PROJECT TOPIC- NSPECTROPHOTOMETRIC DETERMINATION OF RISPERIDONE AND MOXIFLOXACINBY CHARGE TRANSFER COMPLEXATION USING CHLORANILIC ACID

 

ABSTRACT

A simple, accurate and sensitive spectrophotometric method for the determination of risperidoneand moxifloxacin has been developed. The method was based on the charge – transfercomplexation of the drugs with chloranilic acid to form a purple – coloured complex havingabsorption maximum at 500 nm for risperidone-chloranilic acid complex and 490 nm formoxifloxacin-chloranilic acid complex. Different variables affecting the reaction conditions suchas the concentration of chloranilic acid, and reaction time were studied and optimized. Under theoptimal conditions, linear relationships between absorbance and concentrations of the drugswith good correlation coefficient (0.996 and 0.995) were found respectively in the range of 5 –40 μg/ml. The assay limits of detection and quantitation were 0.550 and 1.670 μg/ml forrisperidone and 0.297 and 0.900μg/ml for moxifloxacin respectively. The precision of themethod was satisfactory and the values of relative standard deviations never exceeded 2% andthere was no interference from the excipients commonly present in dosage forms. The proposedmethod was successfully applied to the analysis of risperidone and moxifloxacin in pure andpharmaceutical dosage forms with good accuracy and precision; the recovery percentage rangedfrom 96.35±1.19 to 101.88 ± 0.54 for risperidone and 98.90 ± 1.40 to 102.51± 0.10. The resultsobtained by the developed spectrophotometric method were compared with those obtained by theofficial method in the British Pharmacopoeia for rispridone and other methods of analysingmoxifloxacin.

CHAPTER ONE

1.0 INTRODUCTION

1.1.0 SPECTROSCOPYSpectroscopy

involves the study of the absorption, emission of light and other radiation asrelated to the wavelength of the radiation1. Spectroscopy deals with the production, measurementand interpretation of spectra arising from the interaction of electromagnetic radiation withmatter. There are many different spectroscopic methods available for solving a wide range ofanalytical problems. The methods differ with respect to the species to be analyzed (such asmolecular or atomic spectroscopy), the type of radiation – matter interaction to be monitored(such as absorption, emission or diffraction) and the region of the electromagnetic spectrum usedin the analysis.

Spectroscopic methods are very informative and widely used for both quantitative and qualitative analysis2. It has tremendous practical applications in many technicalfields especially in the identification of the constituents of organic compounds. In typicalanalysis, a known concentration of a few parts per million (ppm) of the compound can bedetected and the structure of the compound can thus be ascertained1.Spectroscopic methods are based on the absorption or emission of radiation in the ultraviolet(UV), visible (Vis), infrared (IR) and radio (nuclear magnetic resonance, NMR) frequencyranges. These methods monitor different types of molecular and / or atomic transitions.

Spectroscopic method is classified into photometry and spectrophotometry. Photometry simplymeans light measurement that depends upon the measurement of the amount of light absorbed bya solution (spectrophotometry) or by a suspension (turbidimetry) or the amount of light scatteredby a suspension (nephelometry) or the intensity of light emitted by an element when subjected to high temperature (flame photometry).

The measurement of light in the visible region(colorimetry) may be accomplished using a colorimeter or spectrophotometer or comparisonwith colour standards3. Spectrophotometry is more sophisticated and has much widerapplications than photometry. It involves the use of instruments, a spectrometer and aphotometer, both housed in one cabinet. Light of a spectrophotometer which could be describedessentially as a combination of photometer (a visual, photographic, or photoelectricinstrument for measuring absolute or relative light intensities) with a monochromator (aninstrument for isolating light of a single wavelength)4. Unlike light filter which can only isolatethe required range of wavelengths needed for an analysis, a monochromator can isolate anextremely narrow bandwidth almost comparable to a single wavelength, thereby extending range of application of spectrophotometers from the ultraviolet (185 – 400nm) through visible (400 –760nm) to the infrared (>760nm) region.

PROJECT TOPIC- NSPECTROPHOTOMETRIC DETERMINATION OF RISPERIDONE AND MOXIFLOXACINBY CHARGE TRANSFER COMPLEXATION USING CHLORANILIC ACID

1.1.1 THEORY AND IMPORTANCE OF UV-VISIBLE SPECTROPHOTOMETRY

In ultraviolet and visible spectroscopy, absorption of radiation is the result of excitation ofbonding electrons5. When a molecule absorbs ultraviolet or visible light of frequency, v andwavelength , an electron undergoes a transition from a lower to a higher energy level in themolecule6. The energy difference (E) is related to frequency and wavelength by the expression; whereh is Planck’s constant and c is the velocity of radiation. For the region 200-750nm, theenergy required for electron transition is in the range of 600-160KJmol-1 (multiplication of theexpression by Avogadro’s number will express the energy absorbed per mole).

Energies of thesemagnitude are associated with the promotion of an electron from a non-bonding (n) orbital or a  orbital to an antibonding -orbital (*) or to an antibonding -orbital (*). It therefore, followsthat electronic transitions in organic molecules could be ascribed to a  or  n.The energy required for the transitions of the  electron is much more (usually in far UV) thanthe n-electron or less tightly bonded  electrons. They are seen in the vacuum-UV and harder toobserve. The types of bonds that give rise to UV-Visible absorptions are known aschromophores.

In the ultraviolet, the electrons of the chromophores are either directly used inbond formation or are non-bonding or unshared outer electrons of an electronegative atom suchas oxygen,nitrogen or sulphur5. The most important transitions in organic compound are asfollow:a) transitionThese are usually associated with the multiple bonds of carbon with carbon, nitrogen oxygen,and sulphur. They generally give rise to high intensity absorptions.b) n * transitionThese are usually associated with the groups such as carbonyl, thiocarbonyl, and nitrosogroups.

Generally the intensity of these absorptions are very much lower and lie at longerwavelengths than those arising from  * transitions. However,  * and n *transitions are also known to occur.Transition-metal ions absorb in the UV and visible region and the transitions responsible involve4f and 5d electrons of the metals. Alternatively, in some inorganic complexes, the process ofchange-transfer absorption occurs.Most applications of ultraviolet and visible spectrophotometry to organic compounds are basedon  and transitions and hence require the presence of chromophoric groups in themolecule. These transitions occur in the region of the spectrum (about 200 to 760nm), which isconvenient to use experimentally.

Visible light consists of electromagnetic radiation in thewavelength range 350-760nm, to which the human eye is sensitive. The wavelength andefficiency of absorption by a substance depend on the structure of the substance and itsenvironment, making it possible to measure the presence or concentration of the substance

1.1.2 SPECTROPHOTOMETRIC METHOD

This method uses spectrophotometer which is an instrument for measuring the intensityof light of various wavelengths transmitted by a solution. The intensity of light is determined byelectric detectors, which convert radiant energy to electrical energy and can therefore eliminatethe need of subjective measurements, by the human eye. This method has a number ofadvantages over other methods these include: the limit of detection is lowered by measuring theabsorption of a solution at the wavelength of maximal absorption; the possibility to avoid orminimize the effect of foreign coloured substances by working at a suitable wavelength andgreater precision.

1.1.3 PRINCIPLES OF SPECTROPHOTOMETRIC METHOD

PROJECT TOPIC- NSPECTROPHOTOMETRIC DETERMINATION OF RISPERIDONE AND MOXIFLOXACINBY CHARGE TRANSFER COMPLEXATION USING CHLORANILIC ACID

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