Validated stability-indicating RP-HPLC assay method for fesoterodine fumarate in pharmaceutical products

IF 0.4 4区 医学 Q4 PHARMACOLOGY & PHARMACY
O. Pınarbaşlı, Tolga Ozbay, G. Gurbetoğlu, Nagehan Sarraçoğlu, A. Doganay
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引用次数: 0

Abstract

The goal of the current study was to develop a precise, sensitive and validated reverse phase HPLC method for determination of fesoterodine fumarate (FST). The current investigation was performed for a stability indicating method in order to obtain both assay and impurity profiles of FST. All the experiment was done on HPLC Shimadzu Prominence 20A having stainless steel ACE5 C18 column with a particle size of 5µm and a dimension of 4.6 mm X 150 mm. The mobile phase was in gradient mode with mobile phase A (0.03M ammonium acetate buffer : acetonitrile : methanol (55:30:15 v/v) pH 3.8) and mobile phase B (water) . The flow rate was 1.2 mL/min and the wavelength 208 nm was selected for detection. This method was validated for linearity and range, accuracy, precision and robustness in accordance with ICH requirements. The retention time of fesoterodine was found as 11.0 min. The main degradation product 5-hydroxymethyltolterodine (5-HMT; active metabolite of FST) and the other process impurities; aldehyde, benzylated hydroxy, tolterodine ester, diester impurities were detected easily at the retention times 3.8, 13.5, 16.7, 21.5, 37.1 minutes, respectively. It was observed that the retention times of the main peak and its impurities were not affected and the selectivity of the method was proved under the applied stress conditions. With this developed method, FST and its impurities can easily be detected. It is also stable, simple, accurate, and completely validated RP-HPLC technique for the analysis of FST and related impurities that meets with ICH standards.
药品中富马酸非索特罗定稳定性指示RP-HPLC测定方法验证
本研究的目的是建立一种精确、灵敏、有效的反相高效液相色谱法测定富马酸非索特罗定(FST)的方法。目前的研究是为了获得FST的测定和杂质谱而进行的稳定性指示方法。所有实验均采用高效液相色谱法(HPLC)进行,柱柱为不锈钢ACE5 C18,粒径为5µm,尺寸为4.6 mm X 150 mm。流动相为梯度模式,流动相为A (0.03M醋酸铵缓冲液:乙腈:甲醇(55:30:15 v/v) pH 3.8),流动相为B(水)。流速为1.2 mL/min,检测波长为208 nm。该方法的线性度、范围、准确度、精密度和鲁棒性均符合ICH要求。fesoterodine的停留时间为11.0 min。主要降解产物5-羟甲基托特罗定(5-HMT;FST活性代谢物)等工艺杂质;醛、苯基化羟基、托特罗定酯、二酯杂质在保留时间分别为3.8、13.5、16.7、21.5、37.1 min时易检出。结果表明,在施加应力条件下,该方法的选择性不受主峰及其杂质的保留时间的影响。该方法可以很容易地检测到FST及其杂质。该方法是一种稳定、简便、准确、经过完全验证的反相高效液相色谱技术,可用于FST及相关杂质的分析,符合ICH标准。
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来源期刊
CiteScore
0.80
自引率
0.00%
发文量
74
审稿时长
6-12 weeks
期刊介绍: The international journal of the Polish Pharmaceutical Society is published in 6 issues a year. The journal offers Open Access publication of original research papers, short communications and reviews written in English, in all areas of pharmaceutical sciences. The following areas of pharmaceutical sciences are covered: Analysis, Biopharmacy, Drug Biochemistry, Drug Synthesis, Natural Drugs, Pharmaceutical Technology, Pharmacology and General. A bimonthly appearing in English since 1994, which continues “Acta Poloniae Pharmaceutica”, whose first issue appeared in December 1937. The war halted the activity of the journal’s creators. Issuance of “Acta Poloniae Pharmaceutica” was resumed in 1947. From 1947 the journal appeared irregularly, initially as a quarterly, then a bimonthly. In the years 1963 – 1973 alongside the Polish version appeared the English edition of the journal. Starting from 1974 only works in English are published in the journal. Since 1995 the journal has been appearing very regularly in two-month intervals (six books a year). The journal publishes original works from all fields of pharmacy, summaries of postdoctoral dissertations and laboratory notes.
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