GC-FID/MS method for the impurity profiling of synthetic d-allethrin

• Published in: Journal of separation science Vol. 27; no. 1-2; pp. 89 - 95
• Main Authors: Bragieri, Matteo, Liverani, Alessandra, Zanotti, Maria Cristina, Borzatta, Valerio, Fiori, Jessica, Cavrini, Vanni, Andrisano, Vincenza
• Format: Journal Article
• Language: English
• Published: Weinheim WILEY-VCH Verlag 01.01.2004; WILEY‐VCH Verlag; Wiley
• Subjects: Analysis; Analytical biochemistry: general aspects, technics, instrumentation; Analytical chemistry; Analytical, structural and metabolic biochemistry; Biological and medical sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; d-Allethrin; Exact sciences and technology; Fundamental and applied biological sciences. Psychology; GC-FID/MS; General pharmacology; Impurity profiling; Ion trap; Medical sciences; Method validation; Pharmacology. Drug treatments; Validation; Insecticide; Impurity; Method validation; Coupled method; Pesticides; Pyrethroids; Purity control; Flame ionization detector; Gas chromatography; Ion trap; Impurity profiling; GC-FID/MS; Mass spectrometry; d-Allethrin
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.200301606

A GC/FID/MS method was developed for the identification and quantification of d‐alle thrin (DA) and its major impurities in commercial samples. Optimisation of the experimental conditions was carried out considering such important requirements as resolution, reproducibility, detection limits of 0.1% (m/m) for the impurities, and short analysis time. Under the optimised final conditions the method was validated for specificity, precision (CV% = 0.133 at 2.10 mg/mL and CV% = 0.035 at 3.00 mg/mL), linearity (0–3.00 μg injected), limits of detection (0.09 ng injected) and quantitation (0.28 ng injected), and robustness. The DA related impurities were identified by using a GC/MS method with ion trap mass detection and also by comparison with synthesised standards. The most abundant impurities were crysolactone, allethrolone, chrysanthemic acid, and chloro‐derivatives of DA.