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Simple and Efficient Solution for Robustness Testing in Gradient Elution Liquid Chromatographic Methods
dc.creator | Sljivić, Jasmina | |
dc.creator | Protić, Ana | |
dc.creator | Malenović, Anđelija | |
dc.creator | Otašević, Biljana | |
dc.creator | Zečević, Mira | |
dc.date.accessioned | 2019-09-02T12:07:39Z | |
dc.date.available | 2019-09-02T12:07:39Z | |
dc.date.issued | 2018 | |
dc.identifier.issn | 0009-5893 | |
dc.identifier.uri | https://farfar.pharmacy.bg.ac.rs/handle/123456789/3208 | |
dc.description.abstract | In this paper, an efficient way for robustness testing of gradient elution liquid chromatographic methods is proposed and tested on model mixtures comprising cilazapril, hydrochlorothiazide, and their degradation products, solutes that differ not only in polarities, but also in solubility and absorption characteristics. In general, the robustness could be tested with respect to various responses: resolution, retention factor, selectivity factor, change of detector response, etc. In chromatographic methods, the separation of the adjacent peaks is mandatory, and, consequently, the resolution is usually used as response. In isocratic elution methods, the resolution threshold depends on many factors, such as sizes of adjacent peaks, peak shapes, and asymmetry factor. At the same time, the situation is even more complex in gradient elution methods, because separation depends on a larger number of parameters, such as gradient profile, column geometry, mobile phase flow rate, column equilibration between gradient runs, etc. To ensure baseline separation, the authors propose application of separation criterion (s) as response and indirect modeling in the robustness evaluation. Examined response in this approach is represented by the difference between the retention time of the beginning of the peak and the retention time of the end of the previously eluting peak of the critical pair. Moreover, the proposed methodology included reusing experiments from the optimization phase to define a robust chromatographic region without increasing the number of experiments. It was shown that method robustness can be easily and efficiently evaluated by this methodology. | en |
dc.publisher | Springer Heidelberg, Heidelberg | |
dc.relation | info:eu-repo/grantAgreement/MESTD/Basic Research (BR or ON)/172033/RS// | |
dc.rights | restrictedAccess | |
dc.source | Chromatographia | |
dc.subject | Liquid chromatography | en |
dc.subject | Robustness testing | en |
dc.subject | Gradient elution | en |
dc.subject | Separation criterion | en |
dc.subject | Indirect modeling | en |
dc.title | Simple and Efficient Solution for Robustness Testing in Gradient Elution Liquid Chromatographic Methods | en |
dc.type | article | |
dc.rights.license | ARR | |
dcterms.abstract | Маленовић, Aнђелија; Зечевић, Мира; Протић, Aна; Сљивић, Јасмина; Оташевић, Биљана; | |
dc.citation.volume | 81 | |
dc.citation.issue | 8 | |
dc.citation.spage | 1135 | |
dc.citation.epage | 1145 | |
dc.citation.other | 81(8): 1135-1145 | |
dc.citation.rank | M23 | |
dc.identifier.wos | 000439334900002 | |
dc.identifier.doi | 10.1007/s10337-018-3545-x | |
dc.identifier.scopus | 2-s2.0-85047156435 | |
dc.type.version | publishedVersion |