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Mateo-Vivaracho, LauraAuthor

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September 24, 2024
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Fast and fully automated analytical method for the screening of residues of aziridine and 2-chloroethylamine in pharmaceutical active principles

Publicated to: Journal Of Pharmaceutical And Biomedical Analysis. 55 (3): 458-465 - 2011-06-01 55(3), DOI: 10.1016/j.jpba.2011.02.024

Authors: Zapata, Julian; Temprado, Jorge; Mateo-Vivaracho, Laura; Ferreira, Vicente

Affiliations

Univ Zaragoza, Fac Sci, Dept Analyt Chem, Lab Flavor Anal & Enol,Inst Engn Aragon,I3A, E-50009 Zaragoza, Spain - Author

Abstract

A simple, fast and fully automated method for the screening of aziridine (AZD) and 2-chloroethylamine (CEA) in active pharmaceutical ingredients (API) has been developed. The method is based on the in-fiber derivatization of the amines extracted from the sample headspace (previously dissolved or suspended in alkaline water) with 2,3,4,5,6-pentafluorobenzoyl chloride (PFBCl) previously adsorbed in the PDMS/DVB solid phase microextraction (SPME) fiber. The derivatives formed are further desorbed and analyzed in a gas chromatograph with negative ion chemical ionization mass spectrometry (GC-NCI-MS) using methane as reagent gas. The different operational parameters of the procedure have been optimized to get highest sensitivity. The validation of the method, however, revealed a poor repeatability, particularly evident in water-soluble APIs (RSD > 20% for AZD). In spite of that, the low detection limits (1-3 ng g(-1) for AZD and CEA), speed (44 min total analysis time) and automation make that this method can be satisfactorily used as screening tool to accept or reject API batches attending to their volatile amine content and a critical specified value derived from the 1.5 mu g/day Threshold of Toxicological Concern (TTC) and maxima daily dosages. This was shown by analyzing seventy-five fluvoxamine maleate samples containing known levels of AZD and CEA (between 0.05 and 1.05 mu g g(-1)) in intermediate reproducibility conditions to get reliable estimations of precision and linearity. From these data, acceptance, rejection and non-conclusive areas of response are defined for both analytes at different confidence and replication levels using normal statistics. The method was satisfactorily applied to real fluvoxamine maleate samples. (C) 2011 Elsevier B.V. All rights reserved.

Keywords

2-chloroethylamineAccurate quantificationAdsorptionAliphatic-aminesAromatic-aminesAutomationAziridineAziridinesDerivativesDimethylamine dmaEthylaminesGas chromatography-mass spectrometryGas-chromatographyIn fiber derivatizationIndicators and reagentsLimit of detectionPfbcPfbclPharmaceutical preparationsPlasmReproducibility of resultsSecondary-aminesSolid phase microextractionSolid-phase microextractionSpmeVolatile amines

Quality index

Bibliometric impact. Analysis of the contribution and dissemination channel

The work has been published in the journal Journal Of Pharmaceutical And Biomedical Analysis due to its progression and the good impact it has achieved in recent years, according to the agency Scopus (SJR), it has become a reference in its field. In the year of publication of the work, 2011, it was in position , thus managing to position itself as a Q1 (Primer Cuartil), in the category Pharmaceutical Science. Notably, the journal is positioned above the 90th percentile.

Independientemente del impacto esperado determinado por el canal de difusión, es importante destacar el impacto real observado de la propia aportación.

Según las diferentes agencias de indexación, el número de citas acumuladas por esta publicación hasta la fecha 2025-12-15:

  • WoS: 5
  • Scopus: 5
  • Europe PMC: 1

Impact and social visibility

From the perspective of influence or social adoption, and based on metrics associated with mentions and interactions provided by agencies specializing in calculating the so-called "Alternative or Social Metrics," we can highlight as of 2025-12-15:

  • The use of this contribution in bookmarks, code forks, additions to favorite lists for recurrent reading, as well as general views, indicates that someone is using the publication as a basis for their current work. This may be a notable indicator of future more formal and academic citations. This claim is supported by the result of the "Capture" indicator, which yields a total of: 10 (PlumX).

Awards linked to the item

This work has been funded by the Spanish Government, project AGL2007-65139. J.Z. has received a grant from the Universidad de Zaragoza-Banco Santander Central Hispano.