Kale Rupali, Shete Pratiksha, Doifode Dattatray, Chitlange Sohan
Dr. D.Y. Patil Institute of Pharmaceutical Sciences and Research, Department of Pharmaceutics, Pimpri-Chinchwad, India
Dr. D.Y. Patil Institute of Pharmaceutical Sciences and Research, Department of Quality Assurance, Pimpri-Chinchwad, India
Turk J Pharm Sci. 2021 Sep 1;18(4):438-444. doi: 10.4274/tjps.galenos.2020.58897.
This study was aimed to develop and validate the use of reverse-phase high pressure liquid chromatographic method for the estimation of simvastatin (SIM) and mupirocin (MUP) simultaneously.
The chromatographic method developed is optimized for flow rate with the column, solvent, and buffer used and mobile phase ratio, molarity, and pH. The validation of the optimized method and the forced degradation studies of both drugs (under acidic, alkaline, oxidation, heat, light, and neutral conditions) were conducted following the The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines.
Kromasil C18 column (250 mm × 4.6 mm, 5 µm) with ultraviolet detection at 224 nm and acetonitrile/phosphate buffer (30 mM, 70:30 v/v, pH 3.5; adjustment done using orthophosphoric acid) as mobile phase at a flow rate of 1.1 mL/min were observed to provide a good resolution for MUP and SIM at retention times of 2.32±0.008 and 13.55±0.254 min, respectively, with high accuracy (percent recovery was 99.69±0.82 for MUP and 101.10±0.02 for SIM) and linearity in the range of 5-30 µg/mL (r: 0.9969 for MUP and r: 0.9959 for SIM). The diagnostic limit and the lower limit of determination were 0.771±0.234 and 2.338±0.246 μg/mL for MUP and 0.595±0.282 and 1.803±0.334 µg/mL for SIM, respectively. The validated method was used to understand the degradation behavior of both drugs after the forced degradation studies.
The analytical method developed is determined to be specific, sensitive, precise, and accurate for the estimation of MUP and SIM simultaneously in the combined dosage form.
本研究旨在开发并验证一种反相高效液相色谱法，用于同时测定辛伐他汀（SIM）和莫匹罗星（MUP）。
所开发的色谱方法针对流速、所用色谱柱、溶剂、缓冲液以及流动相比例、摩尔浓度和pH进行了优化。按照人用药品注册技术要求国际协调会指南，对优化后的方法进行了验证，并对两种药物（在酸性、碱性、氧化、加热、光照和中性条件下）进行了强制降解研究。
观察到使用Kromasil C18色谱柱（250 mm×4.6 mm，5 µm），在224 nm处进行紫外检测，以乙腈/磷酸盐缓冲液（30 mM，70:30 v/v，pH 3.5；用正磷酸调节）作为流动相，流速为1.1 mL/min时，莫匹罗星和辛伐他汀分别在保留时间2.32±0.008和13.55±0.254 min处具有良好的分离度，准确度高（莫匹罗星的回收率为99.69±0.82，辛伐他汀的回收率为101.10±0.02），在5 - 30 µg/mL范围内呈线性（莫匹罗星的r为0.9969，辛伐他汀的r为0.9959）。莫匹罗星的诊断限和测定下限分别为0.771±0.234和2.338±0.246 μg/mL，辛伐他汀的分别为0.595±0.282和1.803±0.334 µg/mL。经过强制降解研究后，使用验证后的方法了解了两种药物的降解行为。
所开发的分析方法被确定为在联合剂型中同时测定莫匹罗星和辛伐他汀具有特异性、灵敏性、精密度和准确性。
