التقدير الطيفي لبعض المركبات الفينولية ذوات الاهمية الصيدلانية == Spectrophotometric Determination of Some Phenolic Compounds of Pharmaceutical Importance
Author name:
زينب طالب عبد الكاظم السلطاني
Supervisor name:
قاسم حسن كاظم
General topic:
Chemistry
Specific topic:
Chemistry
Degree:
Master
University:
University of Babylon - College Of Science
Language:
Arabic
University location:
Babylon
First pages:
25T1525 - p.pdf
Abstract:
يتضمن الفصل الاول مقدمة عن تفاعلات الازوتة والازدواج واهميتها وتطبيقاتها في تقدير المستحضرات الصيدلانية، وتضمن ايضا عرضا لبعض الاستخدامات الطبية والصيدلانية للمركبات الفينولية الدوائية المدروسة واستعراضا موجزا للطرائق التحليلية المستخدمة في تقدير المرك | The first chapter included a common introduction on diazotization coupling reaction and their applications to the determination of pharmaceutical preparations. It also included a display of some of its pharmaceutical and medical uses. The chapter also demonstrates a brief review for the analytical methods that have been used for the determination of thymol, Sodium salicylate and Resorcinol in pharmaceutical preparations.The second chapter comprises to describe a simple and sensitive spectrophotometric method for the determination of thymol in aqueous solution, based on the coupling of thymol with diazotized 4 - bromo aniline in strong alkaline medium to produce an intense yellow colored ,water - soluble and stable Azo - dye which exhibits maximum absorption at 464nm. Beer’s law was obeyed between 0.6 - 7.2 µg.ml - 1, with a molar absorptivity of 3.0284×104 l.mol - 1.cm - 1,average recovery was 100.002%, and RSD was 0.796%, the LOD was 0.04?g.ml - 1 and LOQ was 0.1333?g.ml - 1. The method has been applied successfully for the determination of thymol in pharmaceutical preparations (mouthwashes) and the analytical results were compatible with certified value of pharmaceutical preparations and with a standard method. Moreover, the accuracy and validity of the method was evaluated against a standard method using F and t - tests. It was found that experimental F and t values at 95% confidence level did not exceed the critical values indicating that the present proposed methods have a good accuracy and validity. The third chapter demonstrates the development of simple and sensitive spectrophotometric method for the determination of microgram amounts of Sodium salicylate in some of its pharmaceutical preparations based on the coupling and Azo reaction to form an intense shine - yellow, water - soluble dye based on the coupling of Sodium salicylate with diazotized p - amino benzoic acid reagent in strong alkaline medium The dye formed has a maximum absorption at a wavelength of 452 nm. Beer’s law was obeyed between 2 - 30 µg.ml - 1, with a molar absorptivity of 8.5013×103 l.mol - 1.cm - 1, the LOD was 0.06?g.ml - 1 and LOQ was 0.213?g.ml - 1. The method had a good accuracy and precision, since the recovery was 99.702% and the RSD was 0.854%.. The method has been applied successfully in some pharmaceutical preparations including salicylic acid (topical solution). The analytical results agreed well with British pharmacopia method. Moreover, the accuracy and validity of this method were evaluated against pharmacopoeia method using F and t - tests. It was found that experimental F and t values at 95 % confidence level did not exceed the theoretical values indicating that the present method have good accuracy and validity. The fourth chapter comprises the description of a sensitive spectrophotometric method for the determination of resorcinol by diazotization reaction using a diazotized 4 - methoxy aniline reagent in strong alkaline medium, to form brown water - soluble colored dye. Which exhibits maximum absorption at 448 nm. The linear range was between 0.4 - 4.4 µg.ml - 1, with a molar absorptivity of 2.7844×104 l.mol - 1.cm - 1, average recovery of 101.017%, RSD was 1.02%, LOD was 0.019 µg.ml - 1 and LOQ was 0.065 µg.ml - 1. By the application of the proposed method on the some pure types resorcinol, it was found that the results agreed well with British pharmacopeia method. Moreover, the accuracy and validity of this method were evaluated against pharmacopoeia method using F andt - tests. It was found that experimental F and t values at 95 % confidence level did not exceed the theoretical values indicating that the present method have good accuracy and validity.
