一种用于测定原料药和片剂中阿托伐他汀及其杂质的高效液相色谱法。

An HPLC method for the determination of atorvastatin and its impurities in bulk drug and tablets.

作者信息

Ertürk Sidika, Sevinç Aktaş Esra, Ersoy Lale, Fiçicioğlu Samiye

机构信息

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

出版信息

J Pharm Biomed Anal. 2003 Dec 4;33(5):1017-23. doi: 10.1016/s0731-7085(03)00408-4.

DOI:10.1016/s0731-7085(03)00408-4

PMID:14656592

Abstract

A simple high-performance liquid chromatographic (HPLC) method was developed for the analysis of atorvastatin (AT) and its impurities in bulk drug and tablets. This method has shown good resolution for AT, desfluoro-atorvastatin (DFAT), diastereomer-atorvastatin (DSAT), unknown impurities and formulation excipients of tablets. A gradient reverse-phase HPLC assay was used with UV detection. Some solvent systems prepared using methanol or acetonitrile and water or buffer systems with different pH values were tested. Capacity factors of related substances were calculated at all tested systems. Best resolution has been determined using a Luna C18 column with acetonitrile-ammonium acetate buffer pH 4-tetrahydrofuran (THF) as mobile phase. Samples were eluted gradiently with the mobile phase at flowrate 1.0 ml min(-1) and detected at 248 nm. The proposed method was applied to the determination of impurities and were found to contain 0.057-0.081, 0.072-0.097, 0.608-0.664% of the DFAT, DSAT and total impurity, respectively.

摘要

开发了一种简单的高效液相色谱（HPLC）方法，用于分析原料药和片剂中的阿托伐他汀（AT）及其杂质。该方法对AT、去氟阿托伐他汀（DFAT）、非对映体阿托伐他汀（DSAT）、未知杂质和片剂的制剂辅料具有良好的分离度。采用梯度反相HPLC法并结合紫外检测。测试了一些使用甲醇或乙腈与水或不同pH值缓冲体系配制的溶剂系统。计算了所有测试体系中相关物质的容量因子。使用Luna C18柱，以乙腈-醋酸铵缓冲液pH 4-四氢呋喃（THF）作为流动相，确定了最佳分离度。样品用流动相以1.0 ml min(-1)的流速进行梯度洗脱，并在248 nm处检测。该方法应用于杂质的测定，发现DFAT、DSAT和总杂质的含量分别为0.057-0.081%、0.072-0.097%、0.608-0.664%。