Journal of Chromatography B, 794 (2003) 389–395 www.elsevier.com / locate / chromb Short communication Triazinic herbicide determination by gas chromatography–mass spectrometry in breast milk a a a b c a L. Balduini , M. Matoga , E. Cavalli , E. Seilles , D. Riethmuller , M. Thomassin , a, * Y.C. Guillaume a ´ ´ Equipe Sciences Separatives et Biopharmaceutiques (2SB) / Laboratoire de Chimie Analytique, UFR des Sciences Medicales et Pharmaceutiques,2 Place Saint Jacques, 25030 Besanc ¸on Cedex, France b ˆ ´ ´ ´ Equipe Interaction Hote-Greffon et Ingenierie Cellulaire et Genique en Transplantation / Laboratoire de Therapeutique ´ Immunomoleculaire, Centre Hospitalier Universitaire,1 Boulevard Alexandre Fleming, 25030 Besanc ¸on Cedex, France c ´ ´ Service gynecologie obstetrique, Centre Hospitalier Universitaire,2 Place Saint Jacques, 25030 Besanc ¸on Cedex, France Received 24 February 2003; received in revised form 21 May 2003; accepted 23 May 2003 Abstract A solid-phase extraction procedure using a graphitized carbon black cartridge for extraction and cleaning of a series of five triazines (atrazine, deethylatrazine, deisopropylatrazine, ametryne and prometryne) from breast milk samples was developed. Using a chemometric methodology, the optimisation of both the analysis time and the triazinic herbicide separation by gas chromatography–mass spectrometry (GC–MS) was then carried out with only 18 experiments. Detection and quantification limits for 1 ml breast milk sample were, respectively, 0.3 and 1 ppb for each studied compound. The variation coefficients were less than 5% over the concentration range from 1 to 100 ppb. The accuracy was between 98.63 and 104.62% for each triazinic herbicide. The recovery was between 58.64 and 63.22% for the concentration range from 1 to 100 ppb for each triazinic herbicide. The assay was successfully applied to the analysis of several breast milk samples.  2003 Elsevier B.V. All rights reserved. Keywords: Triazines 1. Introduction Today, use of triazines is the subject of significant concerns because these herbicides (and two desalkyl Since their introduction more than 40 years ago, metabolites of atrazine: deethylatrazine and deiso- triazines have been extensively used in agriculture as propylatrazine) are found not only in plant and soil herbicides. Atrazine, ametryne and prometryne are directly treated, but also in surface and ground applied to corn, soybean, sorghum, vine, legumes waters in the following years and in the cultures and several fruit crops for broadleaf weed control. grown [1,2] as well as in agricultural products as e.g. forage and milk [3–7]. Studying breast milk contamination is important from a health standpoint because lactation can be an *Corresponding author. Tel.: 133-3-8166-5544; fax: 133-3- important process for eliminating triazine compounds 8166-5655. (which are gradually ingested with the diet and E-mail address: yves.guillaume@univ-fcomte.fr (Y.C. Guil- laume). accumulate in adipose tissue) from the human organ- 1570-0232 / 03 / $ – see front matter  2003 Elsevier B.V. All rights reserved. doi:10.1016 / S1570-0232(03)00455-0