Application of restricted-access media column in coupled-column RPLC with UV detection and electrospray mass spectrometry for determination of azole pesticides in urine

Abstract

SummaryTriadimenoJ, triadimefon and tetraconazoJe were simultaneously determined in human urine by coupled-column liquid chromatography with both UV and ES-MS detection. These procedures were validated and the values of some merit figures, such as, linear range, detection limits, precision and recovery, obtained with both methods, are compared. A 5 I~m GFF-II, internal-surface, reversed-phase (ISRP, Pinkerton) column coupled to a 3 I~m reversed-phase, Microsphere C18 column were used. To increase sensitivity a solid-phase extraction step with C18 cartridge was carried outyielding recoveries 80-107% (n = 5) with RSD 3 -8% for the LC-LC-UV method and 88 -108% (n = 5), RSD 5 -11% for the LC-ES-MS method. Limits of detection were 1.5 -3.5 I~g L 1 for LC-LC-UV and 0.5 -1.0 I~g L 1 for LC-ES-MS. The methods were employed to detect and quantify pesticides in urine of pest control operators and non-occupationally exposed subjects.