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离子对和电荷转移络合反应分光光度法测定片剂中甲磺酸多沙唑嗪的含量

Spectrophotometric determination of doxazosin mesylate in tablets by ion-pair and charge-transfer complexation reactions.

作者信息

Aydoğmuş Zeynep, Barla Asli

机构信息

Istanbul University, Faculty of Pharmacy, Department of Analytical Chemistry, 34116, Beyazit, Istanbul, Turkey.

出版信息

J AOAC Int. 2009 Jan-Feb;92(1):131-7.

Abstract

Two accurate, easy spectrophotometric methods for the determination of doxazosin mesylate were described. The first method was based on the formation of ion-pair complexes with the acidic sulfophthalein dyes bromocresol purple (BCP) and bromophenol blue (BPB) in pH 3.3 and 4.5 citrate-phosphate buffer, respectively. The formed complexes were extracted into dichloromethane, and their absorbance was measured at 403 and 410 nm for BCP and BPB, respectively. The second method was based on the charge transfer reaction of the drug as an n-electron donor with either 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) or 7,7,8,8-tetracyanoquinodimethane (TCNQ) as pi-acceptors, to give colored radical anions. The absorbances of products were measured at 457 nm in acetonitrile and 838 nm in methanol for DDQ and TCNQ, respectively. Under the optimum reaction conditions, Beer's law was obeyed with a good correlation coefficient (r = 0.9997-0.9999) in the concentration ranges 3.0-18.0, 3.0-20.0, 15.0-95.0, and 10.0-100.0 microg/mL for the BCP, BPB, DDQ, and TCNQ methods, respectively. Limits of detection of the BCP, BPB, DDQ, and TCNQ methods were 0.314, 0.408, 1.935, and 1.610 microg/mL, respectively. The limits of quantification were 1.045, 1.360, 6.449, and 5.367 microg/mL, respectively. The parameters molar absorptivity, precision, accuracy, recovery, robustness, and stability constant were studied. The proposed methods were successfully applied for determination of the drug in tablets with good accuracy and precision. Statistical comparison of the results with those obtained by a reported method showed good agreement and indicated no significant difference in accuracy and precision.

摘要

描述了两种准确、简便的分光光度法用于测定甲磺酸多沙唑嗪。第一种方法基于在pH 3.3的柠檬酸盐 - 磷酸盐缓冲液中与酸性磺酞类染料溴甲酚紫(BCP)形成离子对络合物,以及在pH 4.5的柠檬酸盐 - 磷酸盐缓冲液中与溴酚蓝(BPB)形成离子对络合物。形成的络合物被萃取到二氯甲烷中,分别在403 nm和410 nm处测量其吸光度,用于BCP和BPB。第二种方法基于药物作为n电子供体与作为π受体的2,3 - 二氯 - 5,6 - 二氰基 - 1,4 - 苯醌(DDQ)或7,7,8,8 - 四氰基对苯二醌二甲烷(TCNQ)发生电荷转移反应,生成有色自由基阴离子。产物的吸光度分别在乙腈中457 nm处和甲醇中838 nm处测量,用于DDQ和TCNQ。在最佳反应条件下,BCP、BPB、DDQ和TCNQ方法在浓度范围分别为3.0 - 18.0、3.0 - 20.0、15.0 - 95.0和10.0 - 100.0 μg/mL时符合比尔定律,相关系数良好(r = 0.9997 - 0.9999)。BCP、BPB、DDQ和TCNQ方法的检测限分别为0.314、0.408、1.935和1.610 μg/mL。定量限分别为1.045、1.360、6.449和5.367 μg/mL。研究了摩尔吸光系数、精密度、准确度、回收率、稳健性和稳定常数等参数。所提出的方法成功应用于片剂中药物的测定,具有良好的准确度和精密度。将结果与报道方法获得的结果进行统计比较,显示出良好的一致性,表明在准确度和精密度方面没有显著差异。

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