Corona Charged Aerosol Detector in studying retention and β-cyclodextrin complex stability using RP-HPLC
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2021
Authors
Đajić, NevenaOtašević, Biljana
Malenović, Anđelija
Zečević, Mira
Holzgrabe, Ulrike
Protić, Ana
Article (Published version)
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Binding between cyclodextrin (CD) cavity and guest molecule in Reversed Phase High-Performance Liquid Chromatography (RP-HPLC) is dynamic process. In general, increasing CD concentration is inducing inclusion complex formation, leading to reduction of analyte's retention time. Consequently, the shortness in retention time is a measure of complex stability in HPLC. However, under certain experimental conditions, the retention of some analytes could be prolonged even when concentration of CD in the mobile phase is increased. In order to reveal the cause of this unexpected retention behavior, the present study was carried on. The model mixture consisted of risperidone, olanzapine and their related impurities, while β-CD was selected among CDs, as in the previous study. In order to achieve fast equilibrium between free analyte and β-CD-analyte complex, β-CD was not added to the mobile phase, but only to the sample. Detection was performed with Corona Charged Aerosol Detector (CAD), suitabl...e for non-chromophoric β-CD. When analyzing olanzapine impurity B-β-CD sample, three peaks were detected, namely free β-CD, β-CD-analyte complex and free analyte. The complex stability constant was calculated employing a modification of the Benesi-Hildebrandt equation and CAD has proven to be useful in complex stability constants assessment if retention of free analyte and β-CD-analyte complex is distinguished. For all other analytes only two peaks could be detected, because free analyte and formed complex are eluting at the same retention time. Under such circumstances, the authors proposed the methodology for calculating stability constants and confirmed its applicability to studied model mixture.
Keywords:
HPLC / β-Cyclodextrin / CAD / Inclusion complexes / Stability constantsSource:
Journal of Pharmaceutical and Biomedical Analysis, 2021, 193Publisher:
- Elsevier B.V.
Funding / projects:
- Ministry of Science, Technological Development and Innovation of the Republic of Serbia, institutional funding - 200161 (University of Belgrade, Faculty of Pharmacy) (RS-MESTD-inst-2020-200161)
DOI: 10.1016/j.jpba.2020.113711
ISSN: 0731-7085
WoS: 000600773600017
Scopus: 2-s2.0-85094938167
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Institution/Community
PharmacyTY - JOUR AU - Đajić, Nevena AU - Otašević, Biljana AU - Malenović, Anđelija AU - Zečević, Mira AU - Holzgrabe, Ulrike AU - Protić, Ana PY - 2021 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/3728 AB - Binding between cyclodextrin (CD) cavity and guest molecule in Reversed Phase High-Performance Liquid Chromatography (RP-HPLC) is dynamic process. In general, increasing CD concentration is inducing inclusion complex formation, leading to reduction of analyte's retention time. Consequently, the shortness in retention time is a measure of complex stability in HPLC. However, under certain experimental conditions, the retention of some analytes could be prolonged even when concentration of CD in the mobile phase is increased. In order to reveal the cause of this unexpected retention behavior, the present study was carried on. The model mixture consisted of risperidone, olanzapine and their related impurities, while β-CD was selected among CDs, as in the previous study. In order to achieve fast equilibrium between free analyte and β-CD-analyte complex, β-CD was not added to the mobile phase, but only to the sample. Detection was performed with Corona Charged Aerosol Detector (CAD), suitable for non-chromophoric β-CD. When analyzing olanzapine impurity B-β-CD sample, three peaks were detected, namely free β-CD, β-CD-analyte complex and free analyte. The complex stability constant was calculated employing a modification of the Benesi-Hildebrandt equation and CAD has proven to be useful in complex stability constants assessment if retention of free analyte and β-CD-analyte complex is distinguished. For all other analytes only two peaks could be detected, because free analyte and formed complex are eluting at the same retention time. Under such circumstances, the authors proposed the methodology for calculating stability constants and confirmed its applicability to studied model mixture. PB - Elsevier B.V. T2 - Journal of Pharmaceutical and Biomedical Analysis T1 - Corona Charged Aerosol Detector in studying retention and β-cyclodextrin complex stability using RP-HPLC VL - 193 DO - 10.1016/j.jpba.2020.113711 ER -
@article{ author = "Đajić, Nevena and Otašević, Biljana and Malenović, Anđelija and Zečević, Mira and Holzgrabe, Ulrike and Protić, Ana", year = "2021", abstract = "Binding between cyclodextrin (CD) cavity and guest molecule in Reversed Phase High-Performance Liquid Chromatography (RP-HPLC) is dynamic process. In general, increasing CD concentration is inducing inclusion complex formation, leading to reduction of analyte's retention time. Consequently, the shortness in retention time is a measure of complex stability in HPLC. However, under certain experimental conditions, the retention of some analytes could be prolonged even when concentration of CD in the mobile phase is increased. In order to reveal the cause of this unexpected retention behavior, the present study was carried on. The model mixture consisted of risperidone, olanzapine and their related impurities, while β-CD was selected among CDs, as in the previous study. In order to achieve fast equilibrium between free analyte and β-CD-analyte complex, β-CD was not added to the mobile phase, but only to the sample. Detection was performed with Corona Charged Aerosol Detector (CAD), suitable for non-chromophoric β-CD. When analyzing olanzapine impurity B-β-CD sample, three peaks were detected, namely free β-CD, β-CD-analyte complex and free analyte. The complex stability constant was calculated employing a modification of the Benesi-Hildebrandt equation and CAD has proven to be useful in complex stability constants assessment if retention of free analyte and β-CD-analyte complex is distinguished. For all other analytes only two peaks could be detected, because free analyte and formed complex are eluting at the same retention time. Under such circumstances, the authors proposed the methodology for calculating stability constants and confirmed its applicability to studied model mixture.", publisher = "Elsevier B.V.", journal = "Journal of Pharmaceutical and Biomedical Analysis", title = "Corona Charged Aerosol Detector in studying retention and β-cyclodextrin complex stability using RP-HPLC", volume = "193", doi = "10.1016/j.jpba.2020.113711" }
Đajić, N., Otašević, B., Malenović, A., Zečević, M., Holzgrabe, U.,& Protić, A.. (2021). Corona Charged Aerosol Detector in studying retention and β-cyclodextrin complex stability using RP-HPLC. in Journal of Pharmaceutical and Biomedical Analysis Elsevier B.V.., 193. https://doi.org/10.1016/j.jpba.2020.113711
Đajić N, Otašević B, Malenović A, Zečević M, Holzgrabe U, Protić A. Corona Charged Aerosol Detector in studying retention and β-cyclodextrin complex stability using RP-HPLC. in Journal of Pharmaceutical and Biomedical Analysis. 2021;193. doi:10.1016/j.jpba.2020.113711 .
Đajić, Nevena, Otašević, Biljana, Malenović, Anđelija, Zečević, Mira, Holzgrabe, Ulrike, Protić, Ana, "Corona Charged Aerosol Detector in studying retention and β-cyclodextrin complex stability using RP-HPLC" in Journal of Pharmaceutical and Biomedical Analysis, 193 (2021), https://doi.org/10.1016/j.jpba.2020.113711 . .