Analytical Chemistry Department, Faculty of Pharmacy, Minia University, Minia, Egypt.
Analytical Chemistry Department, Faculty of Pharmacy, Minia University, Minia, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2018 Mar 5;192:108-116. doi: 10.1016/j.saa.2017.10.065. Epub 2017 Nov 8.
Two simple and sensitive spectrophotometric and spectrofluorimetric methods for the determination of terbutaline sulfate, fenoterol hydrobromide, etilefrine hydrochloride, isoxsuprine hydrochloride, ethamsylate, doxycycline hyclate have been developed. Both methods were based on the oxidation of the cited drugs with cerium (IV) in acid medium. The spectrophotometric method was based on measurement of the absorbance difference (ΔA), which represents the excess cerium (IV), at 317nm for each drug. On the other hand, the spectrofluorimetric method was based on measurement of the fluorescent of the produced cerium (III) at emission wavelength 354nm (λ=255nm) for the concentrations studied for each drug. For both methods, the variables affecting the reactions were carefully investigated and the conditions were optimized. Linear relationships were found between either ΔA or the fluorescent of the produced cerium (III) values and the concentration of the studied drugs in a general concentration range of 2.0-24.0μgmL, 20.0-24.0ngmL with good correlation coefficients in the following range 0.9990-0.9999, 0.9990-0.9993 for spectrophotometric and spectrofluorimetric methods respectively. The limits of detection and quantitation of spectrophotometric method were found in general concentration range 0.190-0.787 and 0.634-2.624μgmLrespectively. For spectrofluorimetric method, the limits of detection and quantitation were found in general concentration range 4.77-9.52 and 15.91-31.74ngmL respectively. The stoichiometry of the reaction was determined, and the reactions pathways were postulated. The analytical performance of the methods, in terms of accuracy and precision, were statistically validated and the results obtained were satisfactory. The methods have been successfully applied to the determination of the cited drugs in their commercial pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent agreement and proved that no significant difference in the accuracy and precision.
两种简单而灵敏的分光光度法和荧光光度法已被开发用于测定硫酸特布他林、盐酸芬特罗、盐酸依替福林、盐酸异舒普林、氨甲环酸、盐酸多西环素。这两种方法都是基于铈（IV）在酸性介质中氧化这些药物。分光光度法基于测量每种药物在 317nm 处的吸光度差（ΔA），表示过量的铈（IV）。另一方面，荧光光度法基于测量产生的铈（III）的荧光，发射波长为 354nm（λ=255nm），用于研究每种药物的浓度。对于这两种方法，都仔细研究了影响反应的变量，并优化了条件。在一般浓度范围为 2.0-24.0μgmL、20.0-24.0ngmL 时，发现要么ΔA 或产生的铈（III）值的荧光值与研究药物的浓度之间存在线性关系，并且相关系数在以下范围内均良好，分光光度法和荧光光度法分别为 0.9990-0.9999 和 0.9990-0.9993。分光光度法的检测限和定量限一般在浓度范围内分别为 0.190-0.787 和 0.634-2.624μgmL。对于荧光光度法，检测限和定量限一般在浓度范围内分别为 4.77-9.52 和 15.91-31.74ngmL。确定了反应的化学计量比，并提出了反应途径。该方法的分析性能（准确度和精密度）经统计学验证，结果令人满意。该方法已成功应用于其商业药物制剂中这些药物的测定。与参考方法的结果进行统计比较表明，准确性和精密度没有显著差异。
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