This study focused on the Analytical Quality by Design (AQbD) optimization of the chromatographic separation and mass spectrometric detection of a wide group of structurally heterogeneous model pharmaceutical compounds (PhCs) and transformation products (TPs), chosen to cover the challenging issues of the co-presence of compounds characterized by (i) a wide range of physicochemical properties, (ii) the same mass transitions, and (iii) different ionisation modes. Italian consumption of PhCs were also considered as election criteria of target analytes. C18 and PFP stationary phases, ACN/CH3OH ratios and acidity of the eluents, column temperature, initial organic phase percentage, and elution gradient were investigated by AQbD, aiming at optimizing critical resolutions, sensitivities, and analysis time. Statistically significant models were obtained in most cases with fitting and cross validation coefficients in the ranges of 0.681-0.998 and 0.514-0.967, respectively. After optimization, the analysis of PhCs was performed in a single chromatographic run, adopting a mixed acquisition mode based on scheduled acquisition windows comprising both single polarity and continuous polarity switching. For most investigated PhCs, the method provided detection limits in the sub-ng/L to low ng/L range, meeting for macrolides the sensitivity requested by 2018/840/EU. The optimized method was applied to the direct injection analysis of PhCs and TPs in four wastewater treatment plant (WWTP) effluents and surface water (SW) samples collected in the receiving water bodies. Absolute values of matrix effect were found to be far higher than 20% for most target analytes in most samples. Seventeen PhCs and two TPs were quantified in at least one sample, at the wide concentration range of about 1-3200 ng/L

Quality by Design optimization of a LC-MS/MS method for the analysis of heterogeneous pharmaceutical compounds and their screening in water samples / Lapo Renai, Cristina Vanessa Agata Scordo, Ayoub El Ghadraoui, Sergio Santana-Viera, JoséJuan Santana Rodriguez, Serena Orlandini, Sandra Furlanetto, Donatella Fibbi, Dimitra Lambropoulou, Massimo Del Bubba. - ELETTRONICO. - (2022), pp. 0-0. ((Intervento presentato al convegno 26th International Symposium on Separation Sciences.

Quality by Design optimization of a LC-MS/MS method for the analysis of heterogeneous pharmaceutical compounds and their screening in water samples

Lapo Renai;Cristina Vanessa Agata Scordo;Ayoub El Ghadraoui;Serena Orlandini;Sandra Furlanetto;Donatella Fibbi;Massimo Del Bubba
2022

Abstract

This study focused on the Analytical Quality by Design (AQbD) optimization of the chromatographic separation and mass spectrometric detection of a wide group of structurally heterogeneous model pharmaceutical compounds (PhCs) and transformation products (TPs), chosen to cover the challenging issues of the co-presence of compounds characterized by (i) a wide range of physicochemical properties, (ii) the same mass transitions, and (iii) different ionisation modes. Italian consumption of PhCs were also considered as election criteria of target analytes. C18 and PFP stationary phases, ACN/CH3OH ratios and acidity of the eluents, column temperature, initial organic phase percentage, and elution gradient were investigated by AQbD, aiming at optimizing critical resolutions, sensitivities, and analysis time. Statistically significant models were obtained in most cases with fitting and cross validation coefficients in the ranges of 0.681-0.998 and 0.514-0.967, respectively. After optimization, the analysis of PhCs was performed in a single chromatographic run, adopting a mixed acquisition mode based on scheduled acquisition windows comprising both single polarity and continuous polarity switching. For most investigated PhCs, the method provided detection limits in the sub-ng/L to low ng/L range, meeting for macrolides the sensitivity requested by 2018/840/EU. The optimized method was applied to the direct injection analysis of PhCs and TPs in four wastewater treatment plant (WWTP) effluents and surface water (SW) samples collected in the receiving water bodies. Absolute values of matrix effect were found to be far higher than 20% for most target analytes in most samples. Seventeen PhCs and two TPs were quantified in at least one sample, at the wide concentration range of about 1-3200 ng/L
Book of Abstract
26th International Symposium on Separation Sciences
Lapo Renai, Cristina Vanessa Agata Scordo, Ayoub El Ghadraoui, Sergio Santana-Viera, JoséJuan Santana Rodriguez, Serena Orlandini, Sandra Furlanetto, Donatella Fibbi, Dimitra Lambropoulou, Massimo Del Bubba
File in questo prodotto:
File Dimensione Formato  
Scan_BoA_YS14.pdf

Accesso chiuso

Tipologia: Pdf editoriale (Version of record)
Licenza: DRM non definito
Dimensione 1.21 MB
Formato Adobe PDF
1.21 MB Adobe PDF   Visualizza/Apri   Richiedi una copia

I documenti in FLORE sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/2158/1286343
Citazioni
  • ???jsp.display-item.citation.pmc??? ND
  • Scopus ND
  • ???jsp.display-item.citation.isi??? ND
social impact