el Walily A F, Korany M A, el Gindy A, Bedair M F
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Alexandria University, Egypt.
J Pharm Biomed Anal. 1998 Jul;17(3):435-42. doi: 10.1016/s0731-7085(97)00213-6.
Derivative spectrophotometric, colorimetric and high performance liquid chromatographic methods, for the determination of the antihistaminic cetirizine dihydrochloride in tablet form were described. Spectrophotometrically, cetirizine was determined by the measurement of its first (1D) and second (2D) derivative amplitudes at 239 (peak) and 243-233 nm (peak-to-trough), respectively. The aqueous solutions obeyed Beer's law in the concentration ranges of 1.2-10.0 and 0.8-10.0 micrograms ml-1 for 1D and 2D measurements, respectively. The colorimetric procedure was based on measuring the absorbency of the coloured chromogen resulted from the reaction between cetirizine sodium salt in polar solvent (DMF) and chloranil at 556 nm. The relation with concentrations was linear over 120-250 micrograms ml-1. Optimization of the reaction conditions was studied. At the same time, investigation of the complex formed was made with respect to its composition and the associated constant. A simple liquid chromatographic assay has been developed for the determination of cetirizine dihydrochloride in the presence of one of its synthesis precursor (hydroxyzine hydrochloride). A Bondapak-C18 column was used with a mobile phase consisting of acetonitrile/0.01 M ammonium dihydrogen phosphate (32:68, v/v) containing 0.1% w/v tetrabutyl ammonium hydrogen sulphate adjusted to pH 3 with phosphoric acid at a flow rate of 2 ml min-1. With salicylic acid as internal standard, quantitation was achieved with UV detection at 230 nm based on the peak height ratios. Beer's law was obeyed in a concentration range of 3-35 micrograms ml-1 and the regression line equation was derived with a correlation coefficient of 0.9999. The validity of the methods was further confirmed using the standard addition method. The proposed procedures were successfully applied to the determination of cetirizine in bulk and tablet form, with high percentage of recovery, good accuracy and precision.
描述了用于测定片剂形式的抗组胺药盐酸西替利嗪的导数分光光度法、比色法和高效液相色谱法。采用分光光度法时，通过分别测量西替利嗪在239nm（峰）处的一阶（1D）导数幅度和在243 - 233nm（峰 - 谷）处的二阶（2D）导数幅度来测定西替利嗪。对于1D和2D测量，水溶液在浓度范围分别为1.2 - 10.0μg/ml和0.8 - 10.0μg/ml时符合比尔定律。比色法基于测量极性溶剂（DMF）中的西替利嗪钠盐与四氯苯醌在556nm处反应生成的有色发色团的吸光度。浓度在120 - 250μg/ml范围内与浓度呈线性关系。研究了反应条件的优化。同时，对形成的络合物的组成和相关常数进行了研究。已开发出一种简单的液相色谱法用于在其一种合成前体（盐酸羟嗪）存在的情况下测定盐酸西替利嗪。使用Bondapak - C18柱，流动相由乙腈/0.01M磷酸二氢铵（32:68，v/v）组成，其中含有0.1% w/v的硫酸氢四丁铵，用磷酸调节至pH 3，流速为2ml/min。以水杨酸为内标，基于峰高比在230nm处进行紫外检测实现定量。在3 - 35μg/ml的浓度范围内符合比尔定律，得出回归直线方程，相关系数为0.9999。使用标准加入法进一步证实了这些方法的有效性。所提出的方法已成功应用于测定原料药和片剂形式的西替利嗪，回收率高，准确度和精密度良好。
