Development of a novel liquid chromatography - Evaporative light scattering detection method for bacitracins and applications to quality control of pharmaceuticals
Development of a novel liquid chromatography - Evaporative light scattering detection method for bacitracins and applications to quality control of pharmaceuticals
Engineering Village 2
2006 Elsevier Inc.
Accession number: 062910017972
Title: Development of a novel liquid chromatography - Evaporative light scattering detection method for bacitracins and applications to quality control of pharmaceuticals
Authors: Sarri, Artemis K.; Megoulas, Nikolaos C.; Koupparis, Michael A.
Author affiliation: Laboratory of Analytical Chemistry, Department of Chemistry, University of Athens, Panepistimiopolis, Athens, 15771, Greece
Serial title: Analytica Chimica Acta
Abbreviated serial title: Anal. Chim. Acta
Volume: v 573-574
Monograph title: Instrumental Methods of Analysis - IMA 2005
Issue date: Jul 28 2006
Publication year: 2006
Pages: p 250-257
Language: English
ISSN: 0003-2670
CODEN: ACACAM
Document type: Journal article (JA)
Publisher: Elsevier, Amsterdam, 1000 AE, Netherlands
Abstract: A novel liquid chromatography method for the direct determination of bacitracin main components (Bc-A, -B1, -B2 and -B3), a basic, cyclic polypeptide antibiotic, was developed and validated, based on ion pairs formation with trifluoroacetic acid (TFA) and evaporative light scattering detection (ELSD). The selected analytical column was the Waters Nova-pak C8 (3.9 ? 150 mm), for which the optimum (using modified Simplex algorithm) mobile phase was H2O-ACN (73:27, v/v) containing 0.80 ?L mL-1 of TFA, at a flow rate of 1.0 mL min-1. Optimized ELSD parameters were: nebulizing gas (nitrogen) pressure = 3.5 bar, evaporation temperature = 50 ?C, detector gain = 12. Retention time of Bc-B1, -B2, -B3, -A and -F (oxidative degradation product of Bc-A) was 5.3, 5.8, 7.7, 8.7, 15.9 min, respectively, while zinc ions and related peptides were eluted at 1.3-1.9 min. A logarithmic calibration curve was obtained for each component (r > 0.998), while the concentration range of total bacitracin was 30-235 ?g mL-1. Detection limits for the individual components were in the range 1.0-1.6 ?g mL-1. The proposed method was applied for the direct determination of Bc components and related peptides in raw materials and pharmaceutical formulations (tablets, powder and aerosol) without tedious pretreatment (for tablets, a liquid-liquid extraction of magnesium with oxine was required). In the case of matrix interference, synthetic standards containing the same amounts of excipients or the standard addition technique were used. Recovery from spiked commercial formulations was ranged from 96.7% to 101.5% (in respect of total Bc). ? 2006 Elsevier B.V. All rights reserved.
Number of references: 29
Ei main heading: Liquid chromatography
Ei controlled terms: Light scattering - Antibiotics - Drug products - Organic acids - Quality control - Polypeptides - Degradation
Uncontrolled terms: Bacitracins - Evaporative light scattering detection (ELSD) - Trifluoroacetic acid (TFA) - Matrix interference
Ei classification codes: 801 Chemistry - 741.1 Light/Optics - 461.6 Medicine - 804.1 Organic Compounds - 913.3 Quality Assurance & Control - 802.2 Chemical Reactions
Treatment: Theoretical (THR); Experimental (EXP)
DOI: 10.1016/j.aca.2006.05.042
Database: Compendex
Compilation and indexing terms, ? 2006 Elsevier Inc. All rights reserved
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