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

2004; Wiley; Volume: 27; Issue: 1-2 Linguagem: Inglês

10.1002/jssc.200301606

1615-9314

M. Bragieri, Alessandra Liverani, M. Zanotti, Valerio Borzatta, Jessica Fiori, Vanni Cavrini, Vincenza Andrisano,

Biological and pharmacological studies of plants

A GC/FID/MS method was developed for the identification and quantification of d-allethrin (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 microg 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.