Spectrofluorimetric and Spectrophotometric Stability- Iwndicating Methods for the Analysis of Veralipride in Presence of Its Degradants and in Spiked Human Plasma  

作　　者：Salama,Nahla Nour El Din Ahmed Salem,Maissa Yacoub Abd El Halim,Lobna Mohammed Abdel Fattah,Laila EI-Sayed 

机构地区：[1]National Organization for Drug Control and Research(NODCAR),6 Abu Hazem Street,Pyramids Ave,P.O.Box 29,Giza,Egypt [2]Analytical Chemistry Department,Faculty of Pharmacy,Cairo University,Cairo,Egypt [3]Analytical Chemistry Department,Faculty of Pharmacy,Misr University for Science and Technology,6th of October,Egypt

出　　处：《Chinese Journal of Chemistry》2012年第1期183-189,共7页中国化学（英文版）

摘　　要：Spectrofluorimetric and spectrophotometric stability-indicating methods were developed and validated for analysis of veralipride （Ver） in presence of its hydrolytic and oxidative degradants. The spectrofluorimetric method was based on direct measurement of the intrinsic fluorescence of Ver at 366 nm after excitation at 299 nm using sodium lauryl sulfate （SLS） as micelle enhancer. The fluorescence intensity plot was linear over the concentration range 1.0-10.0 pg.mL-1. The high sensitivity of the method allowed its successful application to the analysis of Ver in spiked human plasma. Two other methods were developed. They are based on the oxidative coupling reac- tion of Vet with 3-methyl benzothiazolin-2-one hydrazone （MBTH） hydrochloride in presence of ceric ammonium sulphate in an acidic medium. The first method depends on spectrophotometric measurement of the stable green colored oxidative coupling product at 660 nm. The different experimental parameters affecting the reaction were optimized. Linearity range is 10.0--100.0 ~tgomL-1. The second method depends on a fluorescence quenching effect of Vet on the fluorescence of Ce3＋. The difference in fluorescence intensity was measured at 380 nm after excitation at 300 nm. This method is applicable over the concentration ranges 0.25-2.50 pg-mL-1. The methods were validated according to the ICH guidelines. They were successfully applied for the analysis of Ver in drug substance, drug product and in laboratory prepared mixtures containing different percentages of hydrolytic and oxidative degradants.Spectrofluorimetric and spectrophotometric stability-indicating methods were developed and validated for analysis of veralipride （Ver） in presence of its hydrolytic and oxidative degradants. The spectrofluorimetric method was based on direct measurement of the intrinsic fluorescence of Ver at 366 nm after excitation at 299 nm using sodium lauryl sulfate （SLS） as micelle enhancer. The fluorescence intensity plot was linear over the concentration range 1.0-10.0 pg.mL-1. The high sensitivity of the method allowed its successful application to the analysis of Ver in spiked human plasma. Two other methods were developed. They are based on the oxidative coupling reac- tion of Vet with 3-methyl benzothiazolin-2-one hydrazone （MBTH） hydrochloride in presence of ceric ammonium sulphate in an acidic medium. The first method depends on spectrophotometric measurement of the stable green colored oxidative coupling product at 660 nm. The different experimental parameters affecting the reaction were optimized. Linearity range is 10.0--100.0 ~tgomL-1. The second method depends on a fluorescence quenching effect of Vet on the fluorescence of Ce3＋. The difference in fluorescence intensity was measured at 380 nm after excitation at 300 nm. This method is applicable over the concentration ranges 0.25-2.50 pg-mL-1. The methods were validated according to the ICH guidelines. They were successfully applied for the analysis of Ver in drug substance, drug product and in laboratory prepared mixtures containing different percentages of hydrolytic and oxidative degradants.

关 键 词：veralipride micelle-enhanced fluorescence MBTH validation stability fluorescence quenching Ce3＋ 

分 类 号：TQ464.7[化学工程—制药化工] O614.33[理学—无机化学]