An internal surface reversed phase column for the effective removal of humic acid interferences in the trace analysis of mecoprop in soils with coupled-column RPLC-UV

摘要

In the development of a screening method for the determination of residues of mecoprop in soils involving coupled-column RPLC-UV (228 nm) the cleanup performance of a 5 #mu#m GFF-II internal surface reversed phase (ISRP, Pinkerton) analytical column (50 * 4.6 mm I. D.) as a first column was investigated. In comparison to an analytical C18 column the ISRP column substantially improved the separation between acidic analyte and coextracted humic substances. Under the selected coupled-column conditions soil extracts obtained after hydrolysis with an aqueous alkaline solution, acidifying and centrifugation could be analyzed directly allowing the determination of mecoprop in soils to a level of about 0.02 mg/kg. A rapid concentration step on a 100 mg C18 solid phase extraction (SPE) cartridge was adopted into the procedure providing a limit of detection (S/N = 3) of 0.01 mg/kg of mecoprop in soil. The method was validated by analyzing freshly spiked soil samples and samples with aged residues. In case of freshly spiked samples the overall recovery was 87% (n = 18, spiked level 0.02-8.0 mg/kg) with a repeatability of 6.8% and a reproducibility of 8.3%. No significant decrease of the recovery was observed for samples with aged residues (n = 15, spiked level 0.1 and 8.0 mg/kg) during a storage of 29 days in the refrigerator at about 4 deg C; a storage of 67 days provided a mean recovery of 76% (n = 14, spiked level 8.0 mg/kg).