High Speed Liquid Chromatography for In-Process Control of Sultamicillin

• Published in: Journal of liquid chromatography & related technologies Vol. 31; no. 18; pp. 2794 - 2811
• Main Authors: Gomis, Domingo Blanco, Núñez, Noé Sánchez, Enguita, Pablo Bernad, Abrodo, Pilar Arias, Álvarez, M. Dolores Gutiérrez
• Format: Journal Article
• Language: English
• Published: Colchester Taylor & Francis Group 30-09-2008; Taylor & Francis
• Subjects: Analysis; Biological and medical sciences; General pharmacology; High speed liquid chromatography; In-process control; Medical sciences; Pharmaceutical technology. Pharmaceutical industry; Pharmacology. Drug treatments; Sultamicillin; Reaction intermediate; Validation; Elution; Gradient; Chemical analysis; Impurity; Lactam; HPLC chromatography; Purity control; Sultamicillin; Precursor; High speed liquid chromatography; Penicillin derivatives; Processing control; Antibiotic; Reversed phase chromatography; Ultraviolet detector; Quality control; Simultaneous measurement; In-process control; Antibacterial agent; Degradation product; Quantitative analysis
• ISSN: 1082-6076; 1520-572X
• DOI: 10.1080/10826070802388417

A fast HPLC method has been developed for simultaneous determination of sultamicillin and its synthesis precursors. The analytes are separated in 2.5 min by means of a Kromasil 100 C18 column (50 mm × 2.1 mm i.d., 3.5 µm) at 25°C. The mobile phase (A: 5 mM KH
2
PO
4
and 20 mM KCl adjusted to pH 6.0 with H3PO4 plus 1% THF and B: acetonitrile with 1% THF) was pumped at a flow rate of 0.5 mL min
−1
according to the fast gradient mode: 0-0.9 min, 40% B; 0.9-1.0 min, 85% B; 1.0-2.5 min, 85% B; 2.5-2.6 min, 40% B, 2.6-4.0 min, 40% B. Detection was by ultraviolet absorbance at 205 nm. The method was validated in accordance with the International Conference on Harmonisation (ICH) guidelines, good accuracy, intermediate precision (≤3.8%), and linearity being observed for all compounds. This method is sensitive (limits of detection ranged between 0.1-1.1 mg l
−1
) and selective for quantifying sultamicillin and its synthesis precursors and could be used for in-process control.