Multi-residue method for the determination of 57 Persistent Organic Pollutants in human milk and colostrum using a QuEChERS-based extraction procedure

Luzardo, Octavio P.; Ruiz-Suárez, Norberto; Almeida-González, Maira; Henríquez-Hernández, Luis Alberto; Zumbado, Manuel; Boada, Luis D.
November 2013
Analytical & Bioanalytical Chemistry;Nov2013, Vol. 405 Issue 27, p9523
Academic Journal
Human breast milk represents the best choice for the nutrition of infants. However, in addition to containing beneficial nutrients and antibodies, it can also be considered the best indicator of infant exposure to contaminants. We developed a multi-residue method using a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure and capillary gas chromatography–triple quadrupole mass spectrometry for the determination of 57 persistent organic pollutants, including 23 organochlorine pesticides, 18 polychlorinated biphenyl (PCB) congeners, and 16 polycyclic aromatic hydrocarbons in human milk and colostrum samples. We have used primary secondary amine in the clean-up step as it gave a more efficient separation of the analytes from fat and superior removal of the co-extracted substances compared with gel permeation chromatography. No significant matrix effect was observed for the tested pollutants, and therefore matrix-matched calibration was not necessary. The average recoveries from spiked samples were in the range of 74.8–113.0 %. The precision was satisfactory, with relative standard deviations below 16 %, while values of 0.1–0.4 μg L −1 were established as the limit of quantification for all the target analytes (0.05 and 100 μg L −1). The method was successfully applied to the analysis of 18 human colostrum and 23 mature milk samples. All the samples tested were positive for at least nine different residues, with some samples containing up to 24 contaminants. Remarkably, the contaminants hexachlorobenzene, p,p’-DDE, PCB 138, PCB 180, phenanthrene, fluoranthene, and pyrene were present in 100 % of the colostrum and mature milk samples analyzed.


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