科研之友
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摘要
With the objective of reducing analysis time and maintaining good efficiency, there has been substantial focus on high-speed chromatographic separations. In this work, the development and validation of a rapid, precise and specific stability-indicating ultra performance liquid chromatography (UPLC) method for the determination of flunarizine dihydrochloride (FNH) in bulk drug and tablets is described. The chromatographic separation of the drug was achieved on a Zorbax extend C18, 50 x 4.6 mm, 1.8 mu m UPLC column within a short runtime of 5.0 min with mobile phase consisting of a mixture of triethylamine and formic acid buffer of pH 2.5 and acetonitrile (50:50 v/v). The eluted compound was detected at 254 nm with a UV detector. The newly developed method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 5.0-300 mu g ml(-1) FNH with regression coefficient (r) value of 0.9999. The limit of detection (S/N = 3) was 1.6 mu g ml(-1) and the limit of quantification (S/N = 10) was 4.9 mu g ml(-1). Forced degradation studies were also performed for the drug sample to demonstrate the stability indicating power of the developed UPLC method. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation were used to assess the stability indicating power of the method. The drug was found to be stable in acidic, thermal, hydrolytic and photolytic stress conditions and showed slight degradation in oxidative stress condition and extensive degradation in basic medium.
- 出版日期2013-6
