title: HPLC based method using sample precolumn cleanup for the determination of triazines and thiolcarbamates in hemodialysis saline solutions.
abstract: Solid-phase extraction (SPE) procedures for cleanup and preconcentration followed by HPLC-UV method were investigated for the simultaneous determination of seven low-dosed pesticides in saline concentrates for hemodialysis. The target compounds were ametryn, desmetryn, prometryn, terbutryn, molinate, triallate and butylate. Polyethylene (three different types), teflon, polyurethane and polystyrene, in powder form, were investigated as adsorbents for solid-phase extraction of the analytes from the saline samples. Quantification was performed at 222nm and the analytes were separated on a LiChrosorb RP-18 (5mum, 125mm x 4mm i.d.) column using gradient elution with water/acetonitrile as mobile phase. The duration each chromatographic run was 18min including column reconditioning. The efficiency of the different SPE substrates for retaining the analytes from the highly concentrated saline (HCS) samples was discussed. The best performance was achieved with polystyrene as SPE material considering preconcentration factor, precolumn clogging, reusing capability and similarity between the mobile phases for SPE and HPLC procedures. Analyte concentrations as low as 1mugL(-1) could be determined in spiked HCS samples after preconcentration on polystyrene SPE precolumns. Recoveries between 98.7 and 102.2% were obtained from commercial spiked samples. Detection limits ranging from 4.8 (for prometryn) to 46mugL(-1) (for butylate) were calculated (without preconcentration). The within-day relative standard deviations (n = 9) ranged from 2.3 to 4.8%.
authors.affiliation: Departamento de Quimica, Universidade Federal de Santa Maria, 97111-970 Santa Maria, RS, Brazil.
authors.forename: Paulo C
authors.initials: PC
authors.lastname: do Nascimento
authors.forename: Ana L B
authors.initials: AL
authors.lastname: Rohlfes
authors.forename: Denise
authors.initials: D
authors.lastname: Bohrer
authors.forename: Leandro M
authors.initials: LM
authors.lastname: de Carvalho
authors.forename: Eduardo J
authors.initials: EJ
authors.lastname: Pilau