caa a22 4500 445801557 CHVBK 20180317145142.0 cr unu---uuuuu 170323e20110401xx s 000 0 eng 10.1007/s10337-011-1970-1 doi (NATIONALLICENCE)springer-10.1007/s10337-011-1970-1 Rapid Screening of Volatile Ion-Pair Reagents Using UHPLC and Robust Analytical Method Development Using DoE for an Acetyl Cholinesterase Inhibitor: Galantamine HBr [Elektronische Daten] [Girish Deshpande, Amrendra Roy, N. Rao, B. Rao, J. Rudraprasad Reddy] As over 70% of pharmaceutical compounds are bases, the analysis of these basic compounds by high performance liquid chromatography (HPLC) continues to be of great value and interesting. Acetyl cholinesterase inhibitors (AChEIs), which contain the basic compounds like Rivastigmine tartrate, Galantamine hydrobromide and Donepezil with different polarities, were chosen for the study. A rapid screening of the volatile ion-pairing reagents was performed using modern techniques like ultra high performance liquid chromatography (UHPLC). The experiments were planned using the ‘Design of Experiments' (DoE) approach to identify the LC-MS compatible ion-pair reagent. In this study, Heptafluorobutyric acid (HFBA) has given a very good peak shape with tailing factor at 1.4 and theoretical plates up to ~5,000 were observed, compared to tailing factor at 1.9 and theoretical plates up to ~3,000 with non-volatile ion-pair reagent sodium heptane sulphonate (SHS). Similarly retention with HFBA was optimum as ~5min in short run time method compared to ~13min with SHS. This ion-pair reagent has proved to be good replacement of sodium alkyl sulphonate modifiers. HFBA can also be used for semi-preparative work for isolation of impurities by just evaporating the solvents. It avoids the extraction of other inorganic modifiers. Springer-Verlag, 2011 Ultra high performance liquid chromatography (UHPLC) nationallicence Volatile ion-pair reagents nationallicence Design of experiments (DoE) nationallicence Acetylcholinesterase inhibitor (AChEI) nationallicence Alzheimer's disease (AD) nationallicence Deshpande Girish Custom Pharmaceutical Services, Dr. Reddy's Laboratories Limited, Plot-31/A, Phase-I, IDA, Jeedimetla, 500055, Hyderabad, AP, India aut Roy Amrendra Custom Pharmaceutical Services, Dr. Reddy's Laboratories Limited, Plot-31/A, Phase-I, IDA, Jeedimetla, 500055, Hyderabad, AP, India aut Rao N. Department of Inorganic and Analytical Chemistry, Andhra University, 530 003, Visakhapatnam, India aut Rao B. Department of Inorganic and Analytical Chemistry, Andhra University, 530 003, Visakhapatnam, India aut Rudraprasad Reddy J. Department of Inorganic and Analytical Chemistry, Andhra University, 530 003, Visakhapatnam, India aut Chromatographia Vieweg Verlag 73/7-8(2011-04-01), 639-648 0009-5893 73:7-8<639 2011 73 10337 https://doi.org/10.1007/s10337-011-1970-1 text/html Onlinezugriff via DOI 1 research-article jats NATIONALLICENCE 856 40 https://doi.org/10.1007/s10337-011-1970-1 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Deshpande Girish Custom Pharmaceutical Services, Dr. Reddy's Laboratories Limited, Plot-31/A, Phase-I, IDA, Jeedimetla, 500055, Hyderabad, AP, India aut NATIONALLICENCE 700 1- Roy Amrendra Custom Pharmaceutical Services, Dr. Reddy's Laboratories Limited, Plot-31/A, Phase-I, IDA, Jeedimetla, 500055, Hyderabad, AP, India aut NATIONALLICENCE 700 1- Rao N. Department of Inorganic and Analytical Chemistry, Andhra University, 530 003, Visakhapatnam, India aut NATIONALLICENCE 700 1- Rao B. Department of Inorganic and Analytical Chemistry, Andhra University, 530 003, Visakhapatnam, India aut NATIONALLICENCE 700 1- Rudraprasad Reddy J. Department of Inorganic and Analytical Chemistry, Andhra University, 530 003, Visakhapatnam, India aut NATIONALLICENCE 773 0- Chromatographia Vieweg Verlag 73/7-8(2011-04-01), 639-648 0009-5893 73:7-8<639 2011 73 10337 Metadata rights reserved Springer special CC-BY-NC licence nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-springer