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Spectrophotometric determination of niacin, thiamine, glibenclamide, erythromycin and para amino benzo ic acid using 2, 3 – dichloro – 5, 6 – dicyano – 1, 4 – benzoquinone

Spectrophotometric determination of niacin, thiamine, glibenclamide, erythromycin and para amino benzo ic acid using 2, 3 – dichloro – 5, 6 – dicyano – 1, 4 – benzoquinone

Title page – – – – – – – – – – i Declaration – – – – – – – – – – ii Certification page – – – – – – – – iii Dedication – – – – – – – – – iv Acknowledgement – – – – – – – – v Abstract – – – – – – – – – iv Table of Contents – – – – – – – – ix List of Figures – – – – – – – – – xxii List of Tables – – – – – – – – – xxvii Abbreviations– – – – – – – – – xxxiv

Chapter ONE

INTRODUCTION

1.0Introduction – – – – – – – 1
1.1Charge transfer complexation- – – – – – 1 1.
1.2Analysis of Drugs – – – – – – 2 1.
1.3Justification of the study – – – – – – 6 1.
1.4Problem of the study – – – – – – – 6 1.
1.5Aims and Objectives- – – – – – – – 7 1.
1.6Scope of study- – – – – – – – 8

Chapter TWO

LITERATURE REVIEW

2.0Literature Review – – – – – – – 9
2.1Charge transfer complex – – – – – 9 2.
1.1Marcus theory- – – – – – – – – 11 ix 2.
1.2The one electron redox reaction – – – – – 11 2.
1.3The outer sphere electron transfer- – – – – – 12
2.2Charge transfer transition energy – – – – – 13
2.3Identification of CT bands – – – – – – 13
2.4Spectroscopy – – – – – – – – 14 2.
4.1Different spectroscopic techniques – – – – – 14 2.
4.2Spectrophotometry – – – – – – 15 2.
4.3Major classes of spectrophotometer – – – – – 16 2.
4.4Terms used in U.V spectroscopy – – – – – 16
2.5Absorption laws – – – – – – – 17
2.62,3- dichloro-5,6- dicyano-1, 4- benzoquinone – – – 18 2.
6.1Previous studies on DDQ- – – – – – – 20
2.7Niacin (Pyridine – 3 – Carboxylic acid) – – – – 20 2.
7.1Previous studies on niacin – – – – – 21
2.8Vitamin B1 (Thiamine Hydrochloride) – – – 22 2.
8.1Previous studies on thiamine hydrochloride- – – – 23
2.9Glibenclamide – – – – – – – – 24 2.
9.1Previous studies on glibenclamide – – – – – 25
2.10Erythromycin – – – – – – – – 26 2.
10.1Previous studies on erythromycin – — – – – 26
2.11Para Aminobenzoic acid (PABA) – – – – – 28 2.
11.1Previous studies on PABA — – – – – – 28 x

Chapter THREE

RESEARCH METHODOLOGY

3.0Experimental – – – – – – – – 30
3.1Materials and Methods – – – – – – 30 3.
1.1Drugs used and their sources – – – – – – 30
3.2Preparation of reagents and standard solutions – – – 32 3.
2.1Preparation of 2, 3-dichloro-5, 6- dicyano 1, 4- benzoquinone – – – – – – – 32 3.
2.2Preparation of Standard solution of erythromycin – – – 32 3.
2.3Preparation of standard solution of glibenclamide – – – 32 3.
2.4Preparation of Standard solution of niacin – – – 32 3.
2.5Preparation of standard solutions of paraminobenzoic acid (PABA) – – – – – – – – 33 3.
2.6Preparation of standard solutions of thiamine hydrochloride – – – – – – – 33
3.3Absorption spectra – – – – – – – – 33 3.3.
1.Absorption spectra of 2,3- dichloro -5,6- dicyano -1, 4-benzoquinone – – – – – – – 33 3.3.
2.Absorption spectra of erythromycin – – – – 33 3.
3.3Absorption spectra of glibenclamide – – – – 34 3.
3.4Absorption spectra of thiamine hydrochloride – – – 34 3.
3.5Absorption spectra of niacin – – – – – – 34 3.
3.6Absorption spectra of paraminobenzoic acid – – – 34 3.
4.1Absorption spectra of erythromycin-DDQ complex – – – 34 xi 3.
4.2Absorption spectra of glibenclamide-DDQ complex – – – 34 3.
4.3Absorption spectra of thiamine hydrochloride-DDQ Complex – – – – – – — – 35 3.
4.4Absorption spectra of niacin-DDQ complex – – – 35 3.
4.5Absorption spectra of paraminobenzoic acid–DDQ Complex – – – – – – – – 35
3.5Stoichiometry of complexes – – – – – – 35 3.
5.1Stoichiometry of Erythromycin–DDQ Reaction – – – 35 3.
5.2Stoichiometry of Glibenclamide – DDQ Reaction – – – 36 3.
5.3Stoichiometry of Thiamine Hydrochloride – DDQ Reaction- – 36 3.
5.4Stoichiometry of Niacin-DDQ Reaction – – – – 36 3.
5.5Stoichiometry of PABA- DDQ Reaction – – – – 37
3.6Effect of time on the formations of complexes- – – – 37 3.
6.1Effect of time on the formations of erythromycin–DDQ complex – 37 3.
6.2Effect of time on the formation of glibenclamide-DDQ complex – 37 3.
6.3Effect of time on the formation of thiamine hydrochloride-DDQ complex – – – – – 38 3.
6.4Effect of time on the formation of PABA- DDQ Complex – – 38 3.
6.5Effect of time on the formation of niacin- DDQ complex — – 38
3.7Effect of solvents on formation of complexes- – – – 38 3.
7.1Effect of solvents on erythromycin -DDQ complex – – – 38 3.
7.2Effect of solvents on glibenclamide – DDQ complex – – 39 3.
7.3Effect of solvents on complex formation of thiamine hydrochloride – 39 xii 3.
7.4Effect of solvents on niacin – DDQ complex – – – – 39 3.
7.5Effect of solvents on PABA- DDQ complex – – – – 40
3.8Effect of temperature on formation complexes – – – 40 3.
8.1Effect of temperature on erythromycin-DDQ complex – – 40 3.
8.2Effect of temperature on glibenclamide-DDQ complex – – 40 3.
8.3Effect of temperature on thiamine- DDQ complex – – 40 3.
8.4Effect of temperature on niacin- DDQ complex – – – 41 3.
8.5Effect of temperature on PABA- DDQ complex – – – 41
3.9pH study on formation of complexes – – – – – 41 3.
9.1pH study on erythromycin –DDQ complex – – – 41 3.
9.3pH study on glibenclamide-DDQ complex – – – – 41 3.
9.4pH study on thiamine hydrochloride-DDQ complex – – 41 3.
9.5pH study on niacin- DDQ complex – – — – – 42 3.
9.6pH study on PABA-DDQ complex – – — – – 42
3.10Determination of association constant, molar absorptivity, Free energy and Benesi- Hildebrand plot of the complexes- – 42 3.
10.1Benesi–Hildebrand plot of erythromycin-DDQ complex – – 42 3.
10.2Benesi- Hildebrand plot of glibenclamide- DDQ complex – – 42 3.
10.3Benesi – Hildebrand plot of thiamine hydrochloride- DDQ complex – – – – – — – – 43 3.
10.4Benesi – Hildebrand plot of niacin –DDQ complex – – 43 3.
10.5Benesi-Hildebrand plot of PABA-DDQ complex – – – 44
3.2Beer’s calibration plot for the formation of complexes – – 44 xiii
3.21Beer’s calibration plot of erythromycin –DDQ complex – – 44
3.22Beer’s calibration plot of glibenclamide –DDQ complex- – – 44
3.23Beer’s calibration plot of PABA –DDQ complex – – – 45
3.24Beer’s calibration plot of niacin-DDQ complex – – – 45
3.25Beer’s calibration plot of thiamine–DDQ complex – – – 45
3.30Interference studies on complex formation – – – – 46
3.31Interference studies of erythromycin-DDQ complex – – – 46
3.32Interference studies of thiamine hydrochloride-DDQ Complex – 46
3.33Interference studies of niacin –DDQ complex – – – 46
3.34Interference studies of PABA-DDQ complex – – – 47
3.35Interference studies of glibenclamide-DDQ complex – – 47
3.40Assay of dosage forms of drug samples – – – – – 47
3.41Assay of dosage form of erythromycin drug – – – – 48
3.42Assay of dosage form of glibenclamide drug – – – – 48
3.43Assay of dosage form of thiamine drug- – – – – 48
3.44Assay of dosage form of niacin drug – – – – 49
3.45Assay of dosage form of PABA drug – – – – – 49
3.5Kinetic measurements- – – – – – – 50

Chapter FOUR

DATA PRESENTATION AND ANALYSIS

4.
1.1Results – – – – – – – – – 52 4.
1.2Absorption spectra of the complex – – – – – 52
4.20Stoichiometric relationship of erythromycin-DDQ Complex- – 81
4.21Stoichiometric relation of glibenclamide –DDQ complex – – 81 xiv
4.22Stoichiometric relationship of thiamine hydrochloride-DDQ complex – 81
4.23Stoichiometric relationship of niacin-DDQ complex – – – 81
4.24Stoichiometric relationship of PABA- DDQ complex- – – 81
4.30Effect of time on the formation of complex – – – – 95
4.31Maximum time for the formation of erythromycin-DDQ Complex – 95
4.32Effects of time on glibenclamide-DDQ complex – – – 95
4.33Effect of time on thiamine-DDQ complex – — – – 95
4.34Effects of time on niacin-DDQ complex – — – – 95
4.35Effects of time on PABA- DDQ complex – — – – 95
4.40Effect of temperature on complexation- – – – – 108
4.41Effect of temperature on the erythromycin-DDQ Complex – – 108
4.42Effect of temperature on glibenclamide-DDQ Complex – – 108
4.43Effects of temperature on thiamine hydrochloride-DDQ complex – 108
4.44Effects of temperature on niacin-DDQ complex – – – 108
4.45Effect of temperature on PABA- DDQ complex- – – – 109
4.50pH studies of the complexes – – — – – – 120
4.51pH study of erythromycin-DDQ complex — – – – 120
4.52pH study of glibenclamide -DDQ complex – – – – 120
4.53pH study of thiamine hydrochloride-DDQ complex – – – 120
4.54pH study of niacin-DDQ complex – – – – – 120
4.55pH study of PABA-DDQ complex – – – – – 120
4.6Association constant, molar absorptivity, free gibb’s energy, enthalpy and entropy changes of the complexes – – 131 xv 4.
6.1Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the erythromycin-DDQ complex – 131 4.
6.2Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the glibenclamide-DDQ complex – 142 4.
6.3Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the thiamine- DDQ complex – 152 4.
6.4Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the niacin- DDQ complex – 162 4.
6.5Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the PABA- DDQ complex – – 172
4.7Beer’s calibration plots of the complexes – – 182 4.
7.1Beer’s calibration plot for erythromycin-DDQ Complex – – 182 4.
7.2Beer’s calibration plot for glibenclamide – – – – 184 4.
7.3Beer’s calibration plot of thiamine –DDQ complex – – – 186 4.
7.4Beer’s calibration plot for niacin-DDQ complex – – 188 4.
7.5Beer’s calibration plot for PABA-DDQ complex – – – 190 4.
8.1Recovery experiment of erythromycin-DDQ complex – – 192 4.
8.2Recovery experiment of glibenclamide-DDQ complex – – 195 4.
8.3Recovery experiment of thiamine-DDQ complex – – – 197 4.
8.4Recovery experiment of niacin-DDQ complex – – – – 199 4.
8.5Recovery experiment of PABA-DDQ complex – – – 201 4.
9.1Pharmaceutical interference studies on thiamine–DDQ complex – 203 4.
9.2Pharmaceutical interference studies on niacin –DDQ complex – 204 xvi 4.
9.3Pharmaceutical interference studies on glibenclamide–DDQ complex – 205 4.
9.4Pharmaceutical interference studies on PABA–DDQ Complex – 206 4.
9.5Pharmaceutical interference studies on erythromycin-DDQ complex 207
4.10Determination of order of reactions – – – – – 208 4.
10.1Reaction of glibenclamide with DDQ – – – – 208 4.
10.2Reaction of erythromycin with DDQ- – – – – 211 4.
10.3Reaction of niacin with DDQ – – – – – 213 4.
10.4Reaction of PABA with DDQ – – – – – 216 4.
10.5Reaction of thiamine with DDQ – – – – – 219 4.
10.6Effect of temperatures on reaction rate of erythromycin-DDQ complex 222 4.
10.7Effect of temperatures on reaction rate of glibenclamide-DDQ complex 227 4.
10.8Effect of temperatures on reaction rate of niacin-DDQ Complex – 232 4.
10.9Effect of temperatures on reaction rate of PABA-DDQ Complex – 237 4.
10.10Effect of temperatures on reaction rate of thiamine-DDQ Complex 242 4.
10.11Effect of pH1-pH13 on reaction rate of erythromycin-DDQ Complex 248 4.
10.12Effect of pH1-pH13 on reaction rate of glibenclamide-DDQ complex 250 4.
10.13Effect of pH1-pH13 on reaction rate of niacin-DDQ complex – 252 4.
10.14Effect of pH1-pH13 on reaction rate of PABA-DDQ complex – 254 4.
10.15Effect of pH1-pH13 on reaction rate of thiamine – DDQ complex – 256 4.
10.16Effect of hydrogen ion concentration on reaction rate of – – 258 4.
10.17Effect of hydrogen ion concentration on reaction rate of PABA complex- 260 4.
10.18Effect of hydrogen ion concentration on reaction rate of niacin complex – 262
10.19Effect of hydrogen ion concentration on reaction rate of xvii thiamine complex – – – – – – – – 264 4.
10.20Effect of hydrogen ion concentration on reaction rate of erythromycin complex– – – – – – – 266 4.
10.21Effect of ionic strength on erythromycin-DDQ Complex – 268 4.
10.22Effect of ionic strength glibenclamide-DDQ Complex- – – 270 4.
10.23Effect of ionic strength on niacin-DDQ Complex– – — 272 4.
10.24Effect of ionic strength on PABA-DDQ Complex- – – 274 4.
10.25Effect of ionic strength on thiamine-DDQ Complex- – – 276 4.
10.26Rate determining Steps of drugs-DDQ complex – – – 278 4.
10.27Infrared frequencies and tentative assignments for drugs and reagent – 282

Chapter FIVE

SUMMARY, CONCLUSION AND RECOMMENDATIONS

5.0.1 Discussion- – – – – – – – 287 5.
0.2Absorption Spectra- – – – – – – – 287 5.
0.3Absorption spectra of erythromycin complex- – – – 288 5.
0.4Absorption spectra of erythromycin in different solvent- – – 299 5.
0.5Absorption spectra of glibenclamide complex- – – – 290 5.
0.6Absorption spectra of glibenclamide in different solvent – – 291 5.
0.7Absorption spectra of thiamine complex- – – – – 292 5.
0.8Absorption spectra of thiamine in different solvent- – – – 293 5.
0.9Absorption spectra of niacin complex- – – – – 293 5.
0.10Absorption spectra of niacin in different solvent- – – – 294 5.
0.11Absorption spectra of PABA complex- – – – 294 5.
0.12Absorption spectra of PABA in different solvent- – – – 295 xviii
5.1Stoichiometric relationship of erythromycin-DDQ Complex- – 296 5.
1.1Stoichiometric relation of glibenclamide –DDQ complex – – 296 5.
1.2Stoichiometric relationship of thiamine hydrochloride-DDQ complex 296 5.
1.3Stoichiometric relationship of niacin-DDQ complex — – – 297 5.
1.4Stoichiometric relationship of PABA- DDQ complex – – 297
5.2Effect of time on the formation of complex – – – – 297 5.
2.1Maximum time for the formation of erythromycin-DDQ Complex – 297 5.
2.2Effects of time on glibenclamide-DDQ complex – – – 297 5.
2.3Effect of time on thiamine-DDQ complex – – – – 298 5.
2.4Effects of time on niacin-DDQ complex – – – – 298 5.
2.5Effects of time on PABA- DDQ complex – – – – 298
5.3Effect of temperature on complexation – – – – 298 5.
3.1Effect of temperature on the erythromycin-DDQ Complex – – 298 5.
3.2Effect of temperature on glibenclamide-DDQ Complex- – – 299 5.
3.3Effects of temperature on thiamine hydrochloride- DDQ complex – 299 5.
3.4Effects of temperature on niacin-DDQ complex – – – 300 5.
3.5Effect of temperature on PABA- DDQ complex – – – 300
5.4pH studies of the complexes – – – – – – 301 5.
4.1pH study of erythromycin-DDQ complex – – – – 301 5.
4.2pH study of glibenclamide -DDQ complex – – – – 301 5.
4.3pH study of thiamine hydrochloride-DDQ complex – – – 301 5.
4.4pH study of niacin-DDQ complex – – – – – 301 5.
4.5Effect of pH medium on the formation of PABA-DDQ complex – 302 xix
5.5Association constant, molar absorptivity, free Gibb’s energy, enthalpy and entropy changes for the formation of the complexes – – 302 5.
5.1Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the erythromycin-DDQ complex – 302 5.
5.2Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the glibenclamide-DDQ complex – 303 5.
5.3Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the thiamine- DDQ complex – 304 5.
5.4Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the niacin- DDQ complex – 305 5.
5.5Association constant, molar absorptivity, free energy, enthalpy and entropy changes of the PABA- DDQ complex – – – 305
5.6Beer’s calibration plots for the formation of the complexes – – 306 5.
6.1Beer’s calibration plot for the formation of erythromycin – DDQ complex – 306 5.
6.2Beer’s calibration plot for the formation of glibenclamide-DDQ complex – 306 5.
6.3Beer’s calibration plot for the formation of thiamine – DDQ complex – 306 5.
6.4Beer’s calibration plot for the formation of niacin – DDQ complex – 307 5.
6.5Beer’s calibration plot for the formation of PABA – DDQ complex – 307 5.
7.1Recovery studies on the formation of erythromycin-DDQ reaction – 307 5.
7.2Recovery studies on the formation of glibenclamide-DDQ reaction- 307 5.
7.3Recovery studies on the formation of thiamine-DDQ reaction – 308 5.
7.4Recovery studies on the formation of niacin-DDQ reaction – – 308 5.
7.5Recovery studies on the formation of PABA-DDQ reaction- – 308 xx 5.
8.1Interference studies on the formation of thiamine–DDQ complex – 308 5.
8.2Interference studies on the formation of niacin – DDQ complex – 309 5.
8.3Interference studies on the formation of PABA –DDQ complex 311 5.
8.4Interference studies on the formation of PABA –DDQ complex – 313 5.
8.5Interference studies on the formation of erythromycin -DDQ complex 313 5.
8.6Kinetics measurement – – – – – – 315 5.
8.7Determination of order of reactions – – – – – 315 5.
8.8Determination of order of reactions – – – – – 317 5.
8.9Determination of order of reactions – – – – – 318 5.
8.10Determination of order of reactions – – – – – 320 5.
8.11Determination of order of reactions – – – – – 321 5.
8.12FTIR characterization of the complexes – – – – 322 Chapter Six 6.
0.Conclusion and Recommendation- – – – – – 323 References – – – – – – – – – 326 Appendix – – – – – – – – – – 339

Project Abstract

A simple and sensitive spectrophotometric method is described for the assay of the drugs; niacin, glibenclamide, erythromycin, thiamine and 4-aminobenzoic acid. The method is based on charge transfer complexation (CT) reaction of niacin, glibenclamide, erythromycin, thiamine and 4-aminobenzoic acid as n-electron donors with 2,3- dichloro-5,6-dicyno-1,4-benzoquinone(DDQ) as Ð»-electron acceptor in methanol. Intensely coloured charge transfer complexes with niacin (reddish brown, lmax ;464 nm; εmax, 1.02×103 dm3mol-1cm-1) thiamine (reddish brown ,lmax ;474 nm; εmax, 1.08×103 dm3mol-1cm-1), glibenclamide (reddish brown , lmax ;474 nm; εmax,0.99×103 dm3mol- 1cm-1) erythromycin(reddish brown , lmax ;464 nm; εmax, 1.27×103 dm3mol-1cm-1) 4- aminobenzoic acid(reddish brown, lmax ;474nm; εmax, 1.06×103 dm3mol-1cm-1) all in a 11 stoichiometric ratio. Condition for complete reactions and optimum stability of complexes were niacin (70 min, 60 OC) thiamine (25 min, 40 OC), glibenclamide (35 min, 40 OC), erythromycin (15 min, 60 OC) and 4-aminobenzoic acid (15 min, 60 OC) as absorbances of the complexes remained invariant within these conditions. Formation and stability of the complexes of niacin, thiamine, 4-aminobenzoic acid and erythromycin were optimum at pH 8. For glibenclamide pH 2.0 favoured optimum stability and formation. The bands distinguished for the donors to donor-acceptor CT complexes displayed small changes in band intensities and frequency values in the IR spectra ,The –NH2 group vibration occurring at 3609 cm-1 shifted to 3610 cm-1 in thiamine, PABA (3222 cm-1 to 3183 cm-1), Ñµ (N-H) occurring at 3331cm-1 shifted to 3371 cm-1 in glibenclamide, Ñµ(C= N) occurring at 2936 cm-1 shifted to 2944 cm-1 in niacin, Ñµ (CH3-N) occurring at 2948 cm-1 shifted to 2939 cm-1 in erythromycin. The vi vibration Ñµ (C= O) of DDQ observed at 1665 cm-1 shifted to 1669 cm-1 in the CT complex for thiamine, PABA(1665 cm-1 to 1670 cm-1), glibenclamide(1675 cm-1 to 1676 cm-1), erythromycin(1665 cm-1 to 1674 cm-1), niacin(1665 cm-1 to 1655 cm-1) respectively. Adherence to Beer’s Law was within the concentration range for niacin (5- 130 μg/cm3), thiamine (5-80 μg/cm3), glibenclamide (9-100 μg/cm3), erythromycin (5-150 μg/cm3), 4-aminobenzoic acid(5-90 μg/cm3). Limit of detection and quantification of the drugs based on this method is niacin (1.78 and 5.4), thiamine (1.23 and 3.37), glibenclamide (3.47 and 10.5), erythromycin (2.11 and 6.40), 4-aminobenzoic acid (0.55 and 1.67) respectively. Evaluation of the degree of interference by excipients used in the drugs manufactured indicates tolerance to certain concentrations. A detailed study on the interference of different excipients was made. No significant interference was observed in magnesium stearate (30 μg/cm3), Talc (15-25μg/cm3, 35-40 μg/cm3) with thiamine-DDQ complex. There were no significant interference in stearic acid (35 μg/cm3) but tolerable interference was seen in magnesium stearate (20 μg/cm3) and calcium phosphate (15 μg/cm3) with niacin-DDQ complex. For glibenclamide – DDQ complex, no significant interference was seen with calcium phosphate (30 μg/cm3) but there were tolerable interference present in stearic acid (40 μg/cm3). In 4-aminobenzoic acid, no significant interference was observed with magnesium stearate (30 μg/cm3) and talc (35 -40μg/cm3) but tolerable interference was observed in corn starch (15 μg/cm3). Also no significant interference was seen in corn starch (35 μg/cm3) with erythromycin- DDQ complex but there was tolerable interference in talc (10 μg/cm3). The Pearson correlation coefficient for the compliance of the method as regards the pure and commercial forms of niacin, thiamine, glibenclamide, erythromycin and 4-aminobenzoic vii acids are 0.993, 0.977, 0.987, 0.998 and 0.993 respectively which shows significance with p < 0.01. The analysis of variance test revealed the non-significance of niacin, thiamine, glibenclamide, erythromycin and 4-aminobenzoic acid with p > 0.01. The mean percentage recoveries were 98.94 ± 0.016, 96.2 ± 0.016, 98.24 ± 0.011, 107.4 ± 0.023 and 102.35 ± 0.014 for niacin, thiamine, glibenclamide, erythromycin and 4- aminobenzoic acid respectively. Kinetics of the reactions infer that the rate of formation of the CT complexes did not vary significantly with increase in concentration of glibenclamide, erythromycin, thiamine, niacin and 4-aminobenzoic acid indicating likely zeroth order dependence of the rate with respect to concentration of the drugs. However, the linearity of the pseudo-first order plot points to first order dependence of rate on [DDQ].The overall rate equation for the reactions can be given as − Ä±[Ä±Ä±Ä±] Ä±Ä± = Ä±Ä±Ä±Ä± [Ä±Ä±Ä±] Based on the limit of detection and quantification, adherence to Beer-Lambert’s law and low degree of interference, the method is recommended for the analysis of these drugs.

Project Overview

1.0 Introduction 1.1 Charge Transfer Complexation Acceptors are aromatic systems containing electron withdrawing substituents such as nitro, cyano and halogen groups (Foster, 1967). Electron donors are systems that are electron rich (Ajali and Chukwurah, 2001). The interaction between electron donor and electron acceptor results in formation of charge transfer complex (Ajali et al, 2008). The term charge transfer denotes a certain type of complex which results from interaction of an electron acceptor and an electron donor with the formation of weak bonds (Hassib and Issa, 1996). However the nature of the interaction in a charge transfer complex is not a stable chemical bond and is much weaker than covalent forces. It is better characterized as a weak electron resonance. As a result, the excitation energy of this resonance occurs very frequently in the visible region of the electromagnetic spectrum. This produces the usually intense colour characteristic for these complexes. These optical absorption bands are often referred to as charge transfer bands. Molecular interactions between electron donors and acceptors are generally associated with the formation of intensely coloured charge transfer complexes which absorb radiation in the visible region.Charge transfer (CT) complexes have been widely studied (Ezeanokete et al, 2013; Hala et al, 2013; Frag et al, 2011; Ramzin et al, 2012; Farha, 2013). Charge transfer complexes are known to take part in many chemical reactions like addition, substitution and condensation reactions (Van et al, 2006). Donor acceptor properties are prerequisites for the formation of charge transfer complexes. Most drugs have –NH or –NH2 groups which behave as bases (electron donors) and could form complexes with acids (electron acceptor).Various cases have been reported. The charge-transfer complexes formed between the ephedrine (Eph) 2 drug as a donor with picric acid (Pi) and quinol (QL) as Ä±–acceptors have been synthesized in methanol as a solvent at room temperature and spectroscopically studied as shown in scheme 1: HO N CH3 O H2 CH3 OH [(EPh) (QL)] Complex HO OH HO N CH3 H CH3 Quinol Ephedrine + Scheme 1: Interaction of Ephedrine with Quinol to form the charge transfer complex Spectrophotometry is widely used to monitor the progress of reactions and the position of equilibrium. Its measurement is often straight forward to make and the technique is sensitive and precise provided that relevant limitations (such as the regions over which Beer’s law is valid) are recognized. Spectrophotometric technique continues to be the most preferred methods for routine analytical work due to their simplicity and reasonable sensitivity with significant economical advantages (Raza, 2006). 1.1.2: Analysis of Drugs A spectrophotometric method has been employed for the determination of allopuriol using DDQ through charge transfer formation. The absorption spectra of allopuriol-DDQ complex in acetonitrile solvent showed three maxima at (ÊŽmax = 450 nm; ε1 = 1.95 x103 Lmol-1cm-1), 540 nm (ε2 = 0.80 x 103 Lmol-1cm-1) and 580 nm 3 (ε3 = 0.69 x 103 Lmol-1cm-1) with a 1:1 stoichiometric ratio between allopuriol and DDQ. The charge transfer complex formation is shown in scheme 2: Cl O NC NC O Cl N N NH O H Allopurinol DDQ O O Cl Cl HN N N N N NH O Allopurinol -DDQ Charge Transfer Complex + + Scheme 2: Interaction of Allopurinol with DDQ to form the charge transfer complex DDQ (2,3 – dichloro – 5, 6 – dicyano -p- benzoquinone) acts as an oxidizing (Braude et al, 1956) as well as dehydrating agent in synthetic organic chemistry. It is known for its interaction with drugs having donor sites in their structures and form Ion- Pair charge transfer complexes which offers a basis for quantification of drugs (Ghabsha et al, 2007; Vmsi and Gowri, 2008; Rehman et al, 2008; Rahman and Kashif, 2005; Khaled, 2008; Walash, 2004; El-Ragehy et al, 1997). DDQ as π-electron acceptors often forms highly coloured electron-donor, electron-acceptor or CT complexes with various donors which provide the possibility of determination of drugs by spectrophotometric methods. Vitamin B1 (Thiamine) has its chemical name as 2-[3-[(4-Amino-2-methyl- pyrimidin- 5-yl) methyl] -4-methyl – thiazol – 5 – yl] ethanol. Vitamin B1 is a water soluble vitamin. It plays an important biological role in the metabolic process of the carbohydrate in the human body (Khaled, 2008). Previous studies have utilized different techniques for the estimation of thiamine hydrochloride which includes: 4 normal flow injection (Mouayed, 2012), electrochemical analysis method (Akyilmaz and Dinckaya, 2006) high performance liquid chromato graphy (Ghasemi, 2005) spectrofluorimetry (Hassan, 2001) polarimetry. Also direct spectrophotometric method has been described for the determination of thiamine hydrochloride in the presence of its degradation products (Wahbi et al, 1981). Vitamin B3 (Niacin) chemically designated as [pyridine -3- carboxylic acid] is one of the water soluble vitamins of the B-complex. It is an essential vitamin that is widely available in drug and health food stores. Niacin is sometimes prescribed in high dosages to lower cholesterol. People also take niacin supplements because they think niacin helps ease gastrointestinal disturbances. It is widely distributed among plants and animals. Some analytical methods have been developed for determination of niacin which includes HPLC, flow injection TLC (Sarangi et al, 1985) HPTLC (Tiwari, 2010; Zarzycki et al, 1995; Hsieh, 2005). Furthermore, Spectrophotometric methods have been reported for the simultaneous estimation of Atorvastation and niacin based on simultaneous equation and absorbance ratio method (Sawart et al, 2012). PABA [4-aminobenzoic acid] was used as a component of some medicines e.g analgesic or anesthetic preparations, sunscreen agents and bentiromide (Imondi et al, 1972; Cyr et al, 1976; Charles et al, 1977). It is an essential factor for the growth of bacteria. It is possessed of an antisulfanilamide activity (Zhang et al, 2005). Various methods used for the analysis of PABA include HPLC (Zhang et al, 2005) GC (Zhou and Zhang, 1998; Schmidt et al, 1997; Lambropoulon, 2002). Spectrophotometric methods have been used for the determination of PABA; most of the methods are based on diazotization of PABA and coupling the corresponding agent such as Braton Marshall reagent (Othaman and 5 Mansor, 2005), 4–dimethylaminobenzaldehyde (Yamato and Kinoshita, 1979), N-(Inapthyl) ethylediamine dihydrochloride (Fister and Drazin, 1973) and phyloroglucinol (Othaman and Mansor, 2005).Indirect spectrophotometric method for the determination of PABA has been reported (Salvandor et al, 2003).A flow injection spectrophotometric determination of propoxur with diazotized- 4-aminobenzoic acid oxidation (Mirick, 1943) methods has been reported. Erythromycin (3R, 4S, 5S, 6R, 7R, 9R, 11R, 12R, 13S, 14R) – 4-[(2,6-dideoxy -3- Cmethyl- 3-o-methyl-a-L-ribo-hexopy-ransoyl) oxy] – 14 – ethyl – 7 , 12 , 13 – trihydroxy -3,5,7,9,11,13-hexamethyl- 6 – [ ( 3 , 4 , 6 – trideoxy – 3 – dimethylamino–β- D-xylo-hexopyranosyl)-oxy]oxa cyclotetradecane -2, 10- dione is a macrolide antibiotic that has an antimicrobial spectrum similar to or slightly wider than that of penicillin. It has better coverage of a typical organism and occasional used as a prokinetic agent. It inhibits bacterial reproduction but does not kill bacterial cells. Literature revealed different techniques for the analysis of the studied macrolides. The British Pharmacopeia stated the liquid chromatography method for the assay of erythromycin. Other method of analysis includes spectrofluormetry (Pakinaz, 2002) and (Nawal et al, 2006) capillary electrophoresis HPLC (Maria and Britt, 1995; Dubois et al, 2001; Ramakrishna et al, 2005) voltametry (Faryhaly and Mohammed, 2004) microbiological method (Bernabaeu et al, 1999), spectrophotometry (Tasmin et al, 2008; Carlos et al, 2010; Safwan Roula, 2012; Magar et al, 2012). Glibenclamide chemically known as 5-chloro-n-[2-[4[(cyclohexylamino) carbonyl] -amino] sulphonyl] phenyl] –ethyl] -2-methoxy benzamide is a second generation sulphonyl ureas drug widely used in treatment of type 2 diabetic patient (Parmeswararo et al, 2012). The literature survey shows that spectrophotometric methods have been employed for the determination of glibenclamide based on 6 derivatization technique or coupling with another reagent (Nalwaya, 2008), (Bediar et al, 1990; Lopez et al, 2005; Goweri et al, 2005; Martins, et al, 2007; Gianotto et al,2007) High pressure liquid chromatography methods are the most commonly used for the determination of glibenclamide and different methods coupled with UV detection. Fluorescence (Khtri et al, 2001) detection or mass spectrometry (Smgh and Taylor, 1996) .Thin layer chromatography has been employed for the detection of glibenclamide (Kumasak et al, 2005), voltametric method (Radi, 2004). Spectrofluorimetric method have all been reported. Erythromycin, thiamine, niacin, p-Aminobenzoic acid, and glibenclamide are all bases with –NH2 or –NH groups which have donor sites and can form charge transfer complexes. 1.1.3 Justification of the Study In order to solve the problem of fake drugs which is rampart in Nigeria, there is need for a method of drug analysis which is simple, fast and cost effective. However, this new method of analysis will bring about easier analysis of drugs that is simple, fast and of low cost which will invariably reduce importation and manufacture of substandard drugs in Nigeria. Secondly, the new method will solve the problem of interferences caused by drug excipients. 1.1.4: Problem of the Study These drugs are easily adulterated due to their nature and their high demand. This requires that their degree of purity be certified before usage. Also the methods used in determining these drugs like the flow injection spectrophotometric method , High performance liquid chromatography, voltammetry, polarimetry and spectrofluorimetry all require costly equipment, laborious, involve rigid pH control and use large amounts 7 of organic solvents which are expensive, hazardous to health and harmful to the environment. Methods like spectrophotometry based on charge transfer complexation, which are fast, less laborious and economical, are required for the assay of these drugs. 1.1.5 Aims and Objectives The aim of this research was to determine a method based on formation of CT complex between the drugs and DDQ that is simple, fast, economical and less laborious. The objectives of this research are to: (i) establish the degree of CT complex formation between the drugs and DDQ (ii) determine the stability of the CT complexes with respect to time, temperature and pH. (iii) apply the CT complexes in spectrophotometric determinations of the drug (iv) determine the average recoveries of the drugs in pure and commercial forms (v) validate the proposed method using International Conference on Harmonization Guideline. (vi) determination of the kinetic model for the charge transfer complexation reactions. (vii) characterization of the CT complex using Fourier transformer infra red spectrometer. 8 1.1.6: Scope of Study • U.V Absorption spectra • I.R Absorption spectra • Establishment of Ä±-max • Stoichiometric relationships • Optimum conditions(time , temperature , pH) • Establishment of standard curves • Applying the charge transfer complex in the spectrophotometric determination of the drugs • Validation of the proposed method using international conference on harmonization guidelines • Statistical analysis (One-way analysis of variance and Pearson correlation coefficient) • Determination of order of reactions (zero and 1st order) • Characterization of charge transfer complexes using Fourier transformer infra red spectrometer.

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Spectrophotometric determination of niacin, thiamine, glibenclamide, erythromycin and para amino benzo ic acid using 2, 3 – dichloro – 5, 6 – dicyano – 1, 4 – benzoquinone

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