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Liquid chromatography-tandem mass spectrometry for the identification of impurities in d-allethrin samples.
Fiori, J; Bragieri, M; Zanotti, M C; Liverani, A; Borzatta, V; Mancini, F; Cavrini, V; Andrisano, V.
Afiliación
  • Fiori J; Dip. Scienze Farmaceutiche, Via Belmeloro 6, 40126 Bologna, Italy.
J Chromatogr A ; 1099(1-2): 149-56, 2005 Dec 16.
Article en En | MEDLINE | ID: mdl-16188264
A previous GC/MS study highlighting the impurity profile of the synthetic pesticide d-allethrin is extended here to validate and confirm the impurities identity through the development of soft ionisation HPLC-MS methods. To accomplish this, we developed a reverse phase LC-MS analysis in gradient elution with two distinct soft ionisation techniques, the atmospheric pressure ionisation with electrospray source (API-ESI) and the chemical ionisation (APCI). A single quadrupole and an ion trap, which allowed the simultaneous determination of the molecular masses and structural information of the impurities by acquisition of collisionally induced (CID) product ions spectrum and in-source fragmentation, were employed as analysers. Single quadrupole and ion trap analysers resulted perfectly matching in the d-allethrin impurity fragmentation patterns. All the main impurities over 0.1% identified by GC/MS were confirmed. Results indicate that the proposed HPLC/MS method was found appropriate to confirm the presence of impurities such as chrysolactone, chloro allethrin derivatives, allethrolone and chrysanthemic acid, excluding their formation under GC/MS strong ionisation condition.
Asunto(s)
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Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Plaguicidas / Espectrometría de Masas / Cromatografía Líquida de Alta Presión / Aletrinas Tipo de estudio: Diagnostic_studies Idioma: En Revista: J Chromatogr A Año: 2005 Tipo del documento: Article País de afiliación: Italia Pais de publicación: Países Bajos
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Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Plaguicidas / Espectrometría de Masas / Cromatografía Líquida de Alta Presión / Aletrinas Tipo de estudio: Diagnostic_studies Idioma: En Revista: J Chromatogr A Año: 2005 Tipo del documento: Article País de afiliación: Italia Pais de publicación: Países Bajos