建立非水相滴定法和分光光度法测定盐酸缬更昔洛韦原料药及片剂的含量。

Development of non-aqueous titrimetric and spectrophotometric methods for the determination of valganciclovir hydrochloride in bulk drug and tablets.

机构信息

Department of Chemistry, Faculty of Education and Sciences- Rada'a, Al-Baydha University, Al-Baydha, Yemen.

Department of Chemistry, Faculty of Science, Imam Mohammad Ibn Saud Islamic University, Riyadh, Saudi Arabia.

出版信息

Ann Pharm Fr. 2021 Sep;79(5):489-499. doi: 10.1016/j.pharma.2021.01.010. Epub 2021 Feb 4.

DOI:10.1016/j.pharma.2021.01.010

PMID:33548279

Abstract

Two non-aqueous titrimetric and one visible spectrophotometric methods were developed and validated for the determination of valganciclovir hydrochloride (VLGH) in pure drug and tablets. The titrimetric methods were carried out by titrating the VLGH solution in glacial acetic acid with acetous perchloric acid (HClO) in the presence of mercuric acetate and the end point of this titration was being located either visually (method A) or potentiometrically (method B). The spectrophotometric method (method C) was based on the addition of p-dimethylaminobenzaldehyde (DMAB) solution to VLGH solution and the formed yellow condensation product was measured at 420nm. In titrimetric procedures, both the methods A and B were applicable over the range of 4-20mg VLGH, and the calculations were based on a 1:1 reaction stoichiometry (VLGH:HClO). In a spectrophotometric method, Beer's law was valid in a concentration range of 5-50 μg/mL VLGH with the corresponding value of molar absorptivity of 4.43×10L/mol cm for method C. The limits of detection (LOD) and quantification (LOQ) for method C were 0.3 and 0.92μg/mL, respectively. The developed methods were successfully applied to the determination of VLGH in tablets, and the results were statistically compared with those of a reference method by applying Student's t-test and F-test. Further, the validity of the developed methods was confirmed by recovery studies via standard addition technique.

摘要

两种非水滴定法和一种可见分光光度法被开发并验证用于测定盐酸缬更昔洛韦（VLGH）在纯药物和片剂中的含量。滴定法是在醋酸存在下，用醋酸高氯酸（HClO）滴定 VLGH 溶液，该滴定的终点可以通过目测（方法 A）或电位滴定（方法 B）来确定。分光光度法（方法 C）基于将 p-二甲氨基苯甲醛（DMAB）溶液加入 VLGH 溶液中，并在 420nm 处测量形成的黄色缩合产物。在滴定程序中，方法 A 和 B 都适用于 4-20mg VLGH 的范围，计算基于 1:1 的反应计量比（VLGH:HClO）。在分光光度法中，比尔定律在 5-50μg/mL VLGH 的浓度范围内有效，方法 C 的相应摩尔吸光系数为 4.43×10L/mol cm。方法 C 的检测限（LOD）和定量限（LOQ）分别为 0.3 和 0.92μg/mL。所开发的方法成功地应用于片剂中 VLGH 的测定，并通过应用学生 t 检验和 F 检验，将结果与参考方法进行了统计学比较。此外，通过标准加入技术的回收研究验证了所开发方法的有效性。