Conical precolumn as loading buffer for the main column

Ruijten, H. M.; Amsterdam, P. H. van; Bree, H. de

doi:10.1016/s0021-9673(01)97732-5

Cited by 4 publications

(1 citation statement)

References 13 publications

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“…The key factor for the simple and fast analysis is to work out simple and even faster sample pretreatment [16], because soil sample pretreatment for analysis of pesticide residue is usually a quite restricting and laborious operation [e. g. Novaluron1.pdf). Our work was inspired by the articles [17,18] and especially by the approach outlined in the article [17] where an on-line connected conical column was used like an extraction pre-column for isolation of different analytes from biological matrices such as urine, blood plasma, and liver supernatant. Soil column extraction followed by liquid chromatography and electrospray ionization mass spectrometry was devised for the efficient determination of aryloxyphenoxypropionic herbicides in 5 gram soil samples at lg/kg levels by Lagana et al [19].…”

Section: Introductionmentioning

confidence: 99%

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

Rybár¹,

Góra²,

Hutta³

2007

J of Separation Science

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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.

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