用于原料药硫酸阿扎那韦含量测定的稳定性指示反相高效液相色谱法的建立与验证

Development and validation of a stability-indicating RP-HPLC method for estimation of atazanavir sulfate in bulk.

作者信息

Dey S, Subhasis Patro S, Suresh Babu N, Murthy P N, Panda S K

机构信息

Dr. B.C. Roy College of Pharmacy & Allied Health Sciences, Meghnad Saha Sarani, Bidhannagar, Durgapur 713206, West Bengal, India.

Royal College of Pharmacy and Health Sciences, Dist.-Ganjam, Berhampur 760002, Orissa, India.

出版信息

J Pharm Anal. 2017 Apr;7(2):134-140. doi: 10.1016/j.jpha.2013.12.002. Epub 2013 Dec 31.

DOI:10.1016/j.jpha.2013.12.002

PMID:29404029

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5686860/

Abstract

A stability-indicating reverse phase-high performance liquid chromatography (RP-HPLC) method was developed and validated for the determination of atazanavir sulfate in tablet dosage forms using C column Phenomenix (250 mm×4.6 mm, 5 μm) with a mobile phase consisting of 900 mL of HPLC grade methanol and 100 mL of water of HPLC grade. The pH was adjusted to 3.55 with acetic acid. The mobile phase was sonicated for 10 min and filtered through a 0.45 μm membrane filter at a flow rate of 0.5 mL/min. The detection was carried out at 249 nm and retention time of atazanavir sulfate was found to be 8.323 min. Linearity was observed from 10 to 90 μg/mL (coefficient of determination was 0.999) with equation, =23.427+37.732. Atazanavir sulfate was subjected to stress conditions including acidic, alkaline, oxidation, photolysis and thermal degradation, and the results showed that it was more sensitive towards acidic degradation. The method was validated as per ICH guidelines.

摘要

建立了一种稳定性指示反相高效液相色谱（RP-HPLC）法，并对其进行了验证，用于测定片剂剂型中的硫酸阿扎那韦。采用Phenomenix C柱（250 mm×4.6 mm，5μm），流动相由900 mL HPLC级甲醇和100 mL HPLC级水组成。用乙酸将pH值调至3.55。流动相超声处理10分钟，以0.5 mL/min的流速通过0.45μm的膜过滤器过滤。检测波长为249 nm，硫酸阿扎那韦的保留时间为8.323分钟。在10至90μg/mL范围内观察到线性关系（测定系数为0.999），方程为y = 23.427x + 37.732。对硫酸阿扎那韦进行了酸性、碱性、氧化、光解和热降解等强制降解试验，结果表明它对酸性降解更敏感。该方法按照ICH指南进行了验证。