Details

Autor(en) / Beteiligte

• Muñoz, Raybel
• Alvarez-Hernandez, Alejandro
• Ibarra, Israel S
• Guevara-Lara, Alfredo
• Rodriguez, Jose A

Titel

Evaluation of digoxin-boronate ester formation through in-capillary derivatisation-large volume sample stacking-capillary zone electrophoresis

Ist Teil von

• Analytical methods, 2024-06, Vol.16 (23), p.3675-3683

Ort / Verlag

England: Royal Society of Chemistry

Erscheinungsjahr

2024

Quelle

MEDLINE

Beschreibungen/Notizen

• Determination of digoxin through in-capillary derivatisation based on the formation of o -tolyl- and 2-naphthyl-anionic boronate esters in combination with large volume sample stacking-capillary electrophoresis is proposed. The derivatisation reaction was performed at basic pH values to obtain compounds with a charge and chromophore group during the stacking process. After stacking, the species were separated and detected at 225 nm using p -nitrophenol as an internal standard. Stacking and derivatisation parameters such as pre-concentration time, preconcentration voltage and injection time (relation between the analyte and the derivatisation agent) were evaluated using a Box-Behnken design. Under optimal conditions, the proposed method exhibits a linear range of 1.08-50.00 μM with a limit of detection of 0.36 μM; additionally, adequate repeatability and reproducibility was obtained (%RSD ≤ 5.0%). The methodology was validated by comparing it to an HPLC-UV established methodology and was successfully applied for the determination of digoxin in pharmaceutical tablets and blood serum samples, showing a positive performance for these matrices. Digoxin-boronate ester formation through the stacking and separation of species by CZE using boronic acids as derivatisation agents. The methodology is useful for pharmaceutical and biological fluid application.