Restricted access polypyrrole employed in pipette-tip solid-phase extraction for determination of nimodipine and nicardipine in breast milk

• Published in: Analytical methods Vol. 15; no. 17; pp. 273 - 281
• Main Authors: Silva, Camilla F, Nascimento, Clebio Soares, Borges, Keyller Bastos
• Format: Journal Article
• Language: English
• Published: England Royal Society of Chemistry 04.05.2023
• Subjects: Acetonitrile; Adsorbents; Breast milk; Breastfeeding & lactation; Correlation coefficient; Correlation coefficients; Female; Flow rates; Flow velocity; Fourier transforms; High performance liquid chromatography; Humans; Infrared analysis; Infrared spectroscopy; Liquid chromatography; Mathematical analysis; Milk, Human; Nicardipine; Nimodipine; Polymers - chemistry; Polypyrroles; Pyrroles - chemistry; Sample preparation; Scanning electron microscopy; Solid Phase Extraction - methods; Solid phases; Surface analysis (chemical); Thermogravimetric analysis; Wettability
• ISSN: 1759-9660; 1759-9679
• DOI: 10.1039/d3ay00238a

A HPLC-UV method for the determination of nimodipine and nicardipine in breast milk using restricted access polypyrrole as an adsorbent in pipette-tip solid-phase extraction (PT-SPE) has been developed. The chromatographic conditions were a C 18 column (150 mm × 4.60 mm, 5 μm) using methanol : acetonitrile : ultrapure water (55 : 30 : 15, v/v/v) at a flow rate of 1.0 mL min −1 and detection at 236 nm. The adsorbents have been synthesized and characterized by using Fourier-transform infrared spectroscopy, scanning electron microscopy, thermogravimetric analysis, surface analysis, wettability and point zero charge, and were then applied in sample preparation. The main parameters that affect analyte recovery from breast milk by PT-SPE were optimized and the analytical method showed recoveries around 100%, linearity from 3 to 3000 ng mL −1 , and correlation coefficients ( r ) ≥ 0.99 for the two analytes, in addition to adequate precision, accuracy and robustness. Finally, the validated method has been successfully applied in analyses of breast milk from volunteers. A HPLC-UV method for the determination of nimodipine and nicardipine in breast milk using restricted access polypyrrole as an adsorbent in pipette-tip solid-phase extraction (PT-SPE) has been developed.