Skip to Content
Merck
  • Simultaneous extraction and determination of various pesticides in environmental waters.

Simultaneous extraction and determination of various pesticides in environmental waters.

Journal of separation science (2014-10-02)
Zulin Zhang, Thibault Lefebvre, Christine Kerr, Mark Osprey
ABSTRACT

A simple and rapid method was developed for the simultaneous analysis of nine different pesticides in water samples by gas chromatography with mass spectrometry. A number of parameters that may affect the recovery of pesticides, such as the type of solid-phase extraction cartridge, eluting solvent in single or combination and their volumes, and water pH value were investigated. It showed that three solid-phase extraction cartridges (Strata-X, Oasis HLB, and ENVI-18) produced the greatest recovery while ethyl acetate/dichloromethane/acetone (45:10:45, 12 mL) followed by dichloromethane (6 mL) was efficient in eluting target pesticides from solid-phase extraction cartridges. Different water pH values (4-9) did not show a significant effect on the pesticides recovery. The optimized method was verified by performing spiking experiments with a series of concentrations (0.002-10 μg/L) in waters, with good linearity, recovery, and reproducibility for most compounds. The limit of detection and limit of quantification of this optimized method were 0.01-2.01 and 0.02-6.71 ng/L, respectively, much lower than the European Union environmental quality standard for the pesticides (0.1 μg/L) in waters. The proposed method was further validated by participation in an interlaboratory trial. It was then subsequently applied to river waters from north-east Scotland, UK, for the determination of the target pesticides.

MATERIALS
Product Number
Brand
Product Description

Supelco
Simazine solution, 100 μg/mL in methanol, PESTANAL®, analytical standard
Supelco
Cypermethrin, PESTANAL®, analytical standard
Supelco
Ethyl acetate, analytical standard
Sigma-Aldrich
2-Methylpentane, ≥95.0% (GC)
Supelco
Dichloromethane, analytical standard
Sigma-Aldrich
Ethyl acetate, ReagentPlus®, ≥99.8%
Sigma-Aldrich
Triphenyl phosphate, ≥99%
Sigma-Aldrich
2-Methylpentane, ≥99%
Supelco
Permethrin, PESTANAL®, analytical standard
Supelco
2-Methylpentane, analytical standard
Supelco
Dichloromethane, Selectophore, ≥99.5%
Supelco
Atrazine, PESTANAL®, analytical standard
Sigma-Aldrich
Methanol-12C, 99.95 atom % 12C
Supelco
Simazine, PESTANAL®, analytical standard
Supelco
Atrazine, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Cypermethrin, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
2,3-Dimethylphenol, 98%
Sigma-Aldrich
Ethyl acetate, natural, ≥99%, FCC, FG
Sigma-Aldrich
Ethyl acetate, ≥99%, FCC, FG
Supelco
Triphenyl phosphate, analytical standard
Supelco
Atrazine, analytical standard
Sigma-Aldrich
Dichloromethane, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer
Sigma-Aldrich
Ethyl acetate, ACS reagent, ≥99.5%
Supelco
Triphenyl phosphate solution, NMR reference standard, 3 mM in chloroform-d (99.8 atom % D), NMR tube size 5 mm × 8 in.
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Triphenyl phosphate solution, NMR reference standard, 0.0485 M in acetone-d6 (99.9 atom % D)
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Supelco
Methylene Chloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ethyl acetate, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%
Sigma-Aldrich
Ethyl acetate, suitable for HPLC, ≥99.8%