Skip to Content
Merck
  • Novel unbreakable solid-phase microextraction fibers on stainless steel wire and application for the determination of oxadiargyl in environmental and agricultural samples in combination with gas chromatography-mass spectrometry.

Novel unbreakable solid-phase microextraction fibers on stainless steel wire and application for the determination of oxadiargyl in environmental and agricultural samples in combination with gas chromatography-mass spectrometry.

Talanta (2014-07-26)
Ali Es-Haghi, Masoud Baghernejad, Habib Bagheri
ABSTRACT

Sol-gel based solid-phase microextraction fibers supported by a stainless steel wire were fabricated and employed for GC-MS determination of oxadiargyl in real samples. The fibers were based on four compounds with different polarity: polar and non-polar (end-capped) poly(dimethylsiloxane) (PDMS), polyethylene glycol (PEG), and poly(ethylene-propyleneglycol)-monobutyl ether (UCON). For this purpose, the surface of the stainless steel was initially modified by (3-mercaptopropyl) trimethoxysilane. The results of the modification procedure were evaluated by cyclic voltammetry and energy dispersive X-ray (EDX) spectroscopy. After the modification, four different sol-gel based SPME fibers with different values of polarity, polar and non-polar PDMS, PEG, and UCON have been prepared and investigated. They are supposed to be employed to determinate oxadiargyl in agricultural and environmental samples prior to gas chromatography-mass spectrometry analysis. Most important parameters that affect the extraction efficiency were also optimized. Under optimized conditions, the proposed method was found to be linear for the concentrations ranging from 100 ng L(-1) to 2 mg L(-1) with R(2)=0.997. Limit of detection (LOD) of 40 ng L(-1) and relative standard deviation of less than 10% were obtained. Relative recovery in environmental and agricultural samples was in the range of 73-96%.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
Supelco
Methanol, analytical standard
Sigma-Aldrich
Ammonia, puriss., anhydrous, ≥99.95%
Supelco
Acetone, analytical standard
Sigma-Aldrich
Acetone, ≥99%, FCC, FG
Sigma-Aldrich
Poly(dimethylsiloxane), viscosity 1.0 cSt (25 °C)
Sigma-Aldrich
Hexamethyldisiloxane, viscosity 0.65 cSt (25 °C)
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Sigma-Aldrich
Sodium hydroxide, BioUltra, suitable for luminescence, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide solution, BioUltra, Molecular Biology, 10 M in H2O
Sigma-Aldrich
3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
Sigma-Aldrich
Methoxytrimethylsilane, 99%
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Acetone, natural, ≥97%
Sigma-Aldrich
Ammonia solution, 0.4 M in THF
Sigma-Aldrich
Ammonia solution, 4 M in methanol
Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Sigma-Aldrich
Ammonia-14N, 99.99 atom % 14N
Supelco
Dehydrated Alcohol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Acetone, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Sodium hydroxide, ultra dry, powder or crystals, 99.99% trace metals basis
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Acetone, ACS reagent, ≥99.5%
Sigma-Aldrich
Sodium hydroxide, puriss., meets analytical specification of Ph. Eur., BP, NF, E524, 98-100.5%, pellets
Sigma-Aldrich
Sodium hydroxide, reagent grade, 97%, powder
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
Sigma-Aldrich
Sodium hydroxide, pellets, semiconductor grade, 99.99% trace metals basis