Приказ основних података о документу
Generic approach in a gradient elution HPLC method development that enables troubleshooting free method transfer
dc.creator | Milenković, Milan | |
dc.creator | Rašević, Marija | |
dc.creator | Otašević, Biljana | |
dc.creator | Zečević, Mira | |
dc.creator | Malenović, Anđelija | |
dc.creator | Protić, Ana | |
dc.date.accessioned | 2021-10-12T10:38:56Z | |
dc.date.available | 2021-10-12T10:38:56Z | |
dc.date.issued | 2022 | |
dc.identifier.issn | 0731-7085 | |
dc.identifier.uri | https://farfar.pharmacy.bg.ac.rs/handle/123456789/3977 | |
dc.description.abstract | Nowadays, method development is strongly focused on reducing time needed for method development and execution. This subject specially concerns gradient elution methods regarding the usual need for trouble shooting assistance with uncertain outcome during the method transfer from one laboratory to another. One of the main reasons for this situation is the dwell volume difference between HPLC systems. Therefore, the aim of this study was to propose a novel method development methodology that would integrate the dwell volumes differences in the optimization process. The proposed approach could be quite useful in industry that has insight in HPLC instruments planned to be used during the method life cycle. It was tested on the model mixture consisting of dabigatran etexilate mesylate and its nine impurities by use of perimental design methodology. Three different (U)HPLC instruments with high dwell volume differences were selected to challenge the methodology. Plan of experiments was defined with Plackett-Burman design for screening phase and D-optimal design for optimization phase. Initial and final amount of organic modifier, time of the gradient elution and pH value of the aqueous phase were selected as variables nificant for the gradient programme profile and included in the optimization stage along with dwell volume values. The separation criteria s between critical peak pairs was selected as output for method optimization while indirect modelling together with Monte Carlo simulations enabled selection of optimal and robust chromatographic conditions. They included 24% (v/v) of initial amount of acetonitrile, 54% (v/v) of the final amount of acetonitrile, 15 min of gradient elution run time and pH value equal to 4.9. The proposed method was successfully validated, met all validation criteria and thus proved its utility. | |
dc.publisher | Elsevier B.V. | |
dc.relation | info:eu-repo/grantAgreement/MESTD/inst-2020/200161/RS// | |
dc.rights | restrictedAccess | |
dc.source | Journal of Pharmaceutical and Biomedical Analysis | |
dc.subject | (U)HPLC | |
dc.subject | Design of experiments | |
dc.subject | Dwell volume | |
dc.subject | Gradient elution method | |
dc.subject | Method optimization | |
dc.subject | Method transfer | |
dc.title | Generic approach in a gradient elution HPLC method development that enables troubleshooting free method transfer | |
dc.type | article | |
dc.rights.license | ARR | |
dcterms.abstract | Зечевић, Мира; Миленковић, Милан; Оташевић, Биљана; Рашевић, Марија; Маленовић, Aнђелија; Протић, Aна; Генериц аппроацх ин а градиент елутион ХПЛЦ метход девелопмент тхат енаблес троублесхоотинг фрее метход трансфер; | |
dc.citation.volume | 207 | |
dc.citation.rank | M21 | |
dc.identifier.wos | 000706129700009 | |
dc.identifier.doi | 10.1016/j.jpba.2021.114367 | |
dc.identifier.scopus | 2-s2.0-85116113013 | |
dc.type.version | publishedVersion |