DEVELOPMENT AND VALIDATION OF STABILITY-INDICATING TLC-DENSITOMETRIC METHOD FOR DETERMINATION OF BETAXOLOL WITH LC-ESI/MS ANALYSIS OF DEGRADATION PRODUCT

作者：Kwiecien Anna; Krzek Jan^*; Walczak Maria; Mazur Mateusz

来源：Acta Poloniae Pharmaceutica, 2013, 70(4): 643-652.

• betaxolol HCl
• drug analysis
• thin-layer chromatography
• densitometric detection

The purpose of this work was to develop a sensitive stability indicating TLC-densitometric method for the determination of betaxolol (Bx) in pharmaceutical preparations and to study the stability of Bx in acidic solutions. The method was developed on TLC aluminium plates precoated with silica gel F-254 using the mobile phase chloroform-methanol-ammonia 25% (18 : 4 : 0.2, v/v/v) which gives compact spots for Bx (R-f congruent to 0.64) and its degradation product (R-f congruent to 0.39). Densitometric analysis was carried out in UV at 280 nm. The developed method is highly sensitive (LOD = 66.6 ng/spot, LOQ = 200 ng/spot), precise (RSD = 2.73%) and accurate (mean recovery = 100.28% at 100% level). Bx was subjected to acidic and alkaline hydrolysis but degradation was observed only in acidic solutions. The degradation process was described with kinetic and thermodynamic parameters. Based on LC-ESI/MS analysis, it was found that Bx decomposes in acidic solution to produce ethoxyphenoxy-3-[(1-methylethyl)amino]propan-2-ol.

• 出版日期2013-8