Chromatographic analysis and pKa evaluation of active pharmaceutical ingredients in anti-metastatic breast cancer: Green vs. conventional RPLC

---

Kalkır F., Çubuk Demiralay E., Daldal Y. D., Yılmaz H.

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS, cilt.256, sa.256, ss.116671, 2025 (SCI-Expanded, Scopus)

• Yayın Türü: Makale / Tam Makale
• Cilt numarası: 256 Sayı: 256
• Basım Tarihi: 2025
• Doi Numarası: 10.1016/j.jpba.2025.116671
• Dergi Adı: JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
• Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Academic Search Premier, Analytical Abstracts, Aquatic Science & Fisheries Abstracts (ASFA), BIOSIS, Biotechnology Research Abstracts, CAB Abstracts, Chemical Abstracts Core, Chimica, International Pharmaceutical Abstracts, Veterinary Science Database
• Sayfa Sayıları: ss.116671
• Açık Arşiv Koleksiyonu: AVESİS Açık Erişim Koleksiyonu
• Süleyman Demirel Üniversitesi Adresli: Evet

Özet

This study aimed to determine the chromatographic retention and dissociation/protonation constant (pKa) values of lapatinib and tamoxifen, key drugs used in metastatic breast cancer treatment, at 37°C using both conventional and green high-performance liquid chromatography (HPLC) methods. Qualitative analysis was conducted on an XTerra C18 column (250 ×4.6 mm I.D., 5 μm particle size) at a flow rate of 1 mL/min. Hydroorganic mixtures with 45 %, 50 %, 55 %, and 60 % (v/v) organic modifiers were used to evaluate the retention times of the compounds. The compatibility of pKa values pKass" role="presentation" >$\left({}_{𝑠}{}^{𝑠}\mathit{pK}_{𝑎}\right)$ of the compounds in water-organic solvent mixtures obtained from these studies, which were carried out without any significant change in liquid chromatography performance, with the values obtained by the conventional method is remarkable. The pKass" role="presentation" >${}_{𝑠}{}^{𝑠}\mathit{pK}_{𝑎}$ values determined in this study were correlated with the macroscopic parameters of acetonitrile, methanol, ethanol and the pKa (pKaww)" role="presentation" >${}_{𝑤}{}^{𝑤}\mathit{pK}_{𝑎})$values of lapatinib and tamoxifen in water were calculated. The pKaww" role="presentation" >${}_{𝑤}{}^{𝑤}\mathit{pK}_{𝑎}$ values calculated from these studies are compatible with each other and with the literature values. The environmental impact of the study, which was carried out using the green method and the conventional RPLC method, was evaluated using the Green Solvent Selection Tool (GSST), Green Analytical Procedures Index (GAPI), and Analytical Greenness Metric Approach (AGREE).