Development of a Matrix Solid Phase Dispersion methodology for the determination of triazine herbicides in mussels

Abstract

A method based on Matrix Solid Phase Dispersion (MSPD) for determination of nine triazines in mussels has been optimised in terms of the sorbents used for extracting and cleaning-up. Two dispersing agents: C18 and florisil, and eight cleanup co-sorbents: florisil, silica, silica/alumina, Envi™ Carb, Envi-Carb-II/PSA, SAX/PSA, Envi-Carb-II /SAX/PSA and C18 were assayed. Analytes were eluted using 20 mL of ethyl acetate and 5 mL of acetonitrile and finally the extract was concentrated to dryness, re-constituted with 1 mL methanol and determined by HPLC-DAD. The best results were obtained with C18 as dispersing agent and Envi-Carb-II/SAX/PSA as clean-up co-column. Recoveries ranged between 79% and 99% and repeatability and reproducibility were below than 16% for all compounds. The linearity of the calibration curves yielded the R(2)⩾0.9993. The LOQ values ranged from 0.10 to 0.18 mg kg(-1) dried sample. Finally the method was applied to the analysis of mussel samples from Galicia (NW Spain).

Keywords: Ametryn (PubChem CID: 13263); Atrazine (PubChem CID: 2256); Cyanazine (PubChem CID: 30773); Diode array detection; High performance liquid chromatography; Matrix Solid Phase Dispersion; Mussel; Prometryn (PubChem CID: 4929); Propazine (PubChem CID: 4937); Simazine (PubChem CID: 5216); Simetryn (PubChem CID: 13905); Terbuthylazine (PubChem CID: 22206); Terbutryn (PubChem CID: 13450); Triazines.