کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1215709 966981 2006 6 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Micellar electrokinetic chromatography–electrospray ionization mass spectrometry for the identification of drug impurities
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Micellar electrokinetic chromatography–electrospray ionization mass spectrometry for the identification of drug impurities
چکیده انگلیسی

Previously, we have presented a system hyphenating continuous micellar electrokinetic chromatography (MEKC) with electrospray ionization mass spectrometry (ESI-MS). Here we evaluate this technique for its applicability in impurity profiling of drugs using galantamine and ipratropium as test samples. A background electrolyte (BGE) of 10 mM sodium phosphate (pH 7.5), 12.5–15% acetonitrile and 20 mM sodium dodecylsulfate (SDS) was used for the MEKC–MS analysis of a galantamine sample containing a number of related impurities, and a heat-treated solution of ipratropium containing a number of unknown degradation products. MEKC provided efficient separation of all sample constituents. Despite the presence of non-volatile BGEs, all impurities in the galantamine sample could be detected by ESI-MS in their respective extracted ion traces (XICs) with a detection sensitivity in the sub-μg/ml range (full-scan mode). MS/MS detection provided useful product spectra allowing the structural characterization of the respective galantamine impurities. With the MEKC–MS/MS system, two degradation products could be revealed and identified in the heat-stressed ipratropium sample. The presented method shows good potential for the detection and structure elucidation of minor impurities in drug substances.

ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography B - Volume 843, Issue 2, 7 November 2006, Pages 283–288
نویسندگان
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