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  • 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
Chlorpyrifos, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Dichloromethane solution, certified reference material, 5000 μg/mL in methanol
Supelco
Acetone, analytical standard
Supelco
Isoproturon, PESTANAL®, analytical standard
Supelco
α-Cypermethrin, PESTANAL®, analytical standard
Sigma-Aldrich
Acetone, natural, ≥97%
Sigma-Aldrich
Acetone, ≥99%, meets FCC analytical specifications
Supelco
Chlorpyrifos, PESTANAL®, analytical standard
Sigma-Aldrich
Methanol solution, contains 0.50 % (v/v) triethylamine
USP
Acetone, United States Pharmacopeia (USP) Reference Standard
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Acetone, Pharmaceutical Secondary Standard; Certified Reference Material
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Atrazine-d5, PESTANAL®, analytical standard
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Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
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Acetone, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%
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Acetone, suitable for HPLC, ≥99.9%
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Acetone, ACS reagent, ≥99.5%
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Acetone, ACS reagent, ≥99.5%
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Acetone, puriss., meets analytical specification of Ph. Eur., BP, NF, ≥99% (GC)
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Acetone, Laboratory Reagent, ≥99.5%
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Acetone, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.5% (GC)
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Acetone, histological grade, ≥99.5%
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Acetone, suitable for HPLC, ≥99.8%
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Dichloromethane, ACS reagent, ≥99.5%, contains 40-150 ppm amylene as stabilizer
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Ethyl Acetate, Pharmaceutical Secondary Standard; Certified Reference Material
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Methanol, Laboratory Reagent, ≥99.6%
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Methanol, ACS reagent, ≥99.8%
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Methanol, ACS reagent, ≥99.8%
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Ethyl acetate, ACS reagent, ≥99.5%
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Dichloromethane, contains 40-150 ppm amylene as stabilizer, ACS reagent, ≥99.5%