Premium
Method of fast trace microanalysis of the chiral pesticides epoxiconazole and novaluron in soil samples using off‐line flow‐through extraction and on‐column direct large volume injection in reversed‐phase high performance liquid chromatography
Author(s) -
Rybár Ivan,
Góra Robert,
Hutta Milan
Publication year - 2007
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200700180
Subject(s) - chromatography , chemistry , high performance liquid chromatography , extraction (chemistry) , detection limit , analytical chemistry (journal) , soil test , calibration curve , solid phase extraction , soil water , environmental science , soil science
Abstract An analytical method combining off‐line flow‐through extraction of a soil micro‐sample (mass around 100 mg, packed into a short HPLC glass column) and direct on‐column large‐volume injection (LVI up to 1.00 mL) of a methanol–water soil extract onto a conventional C18 RP HPLC column enabled fast (within 3.5 minutes) trace micro‐analysis of the relatively new chiral pesticides epoxiconazole (E) and novaluron (N), respectively. Linear calibration curves were evaluated from UV detection (230 nm) data in the range from 0.1 to 5 mg/kg in three most abundant Slovak agricultural soils. LOD (confidence band) at the levels 0.08–0.11 mg/kg and LOQ 0.4–0.6 mg/kg and LOD ( S/N = 3) at the levels 0.007–0.018 mg/kg and LOQ ( S/N = 10) 0.024–0.060 mg/kg, respectively, of dry soil were achieved. Recovery of pesticides in the overall LVI method including flow‐through 130–200 mg soil micro‐sample extraction was: for epoxiconazole from 74 to 85% and from 56% to 90% for novaluron with reproducibility within ± 6% RSD. This fast (30 min) and simple method consists of just three steps which are short column filling with a solid micro‐sample; flow‐through liquid extraction and direct large‐volume injection RP HPLC DAD analysis. The method is prepared for automation and further analysis of enantiomers of both investigated pesticides by achiral‐chiral column switching techniques.