Skip to Content
MilliporeSigma
  • Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish.

Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish.

Analytical and bioanalytical chemistry (2015-04-26)
Gabriel I Hertzog, Karina L Soares, Sergiane S Caldas, Ednei G Primel
ABSTRACT

A procedure based on vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of 15 pharmaceuticals from fish samples with determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was validated. Florisil, C18, diatomaceous earth, chitin, and chitosan were evaluated as solid supports. Best results were obtained with 0.5 g of diatomaceous earth, 0.5 g of sodium sulfate, and 5 mL of methanol. Analytical recoveries ranged from 58 to 128 % with relative standard deviation (RSD) lower than 15 %. Limit of quantification (LOQ) values for the 15 compounds ranged from 5 to 1000 ng g(-1). The method under investigation has shown to be a simple and fast extraction tool with minimum instrumentation and low amount of reagent, resulting in method low cost. Besides, alternative materials, such as chitin and chitosan, which were applied to the dispersion step for the first time, were found to be interesting alternatives.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol solution, suitable for NMR (reference standard), 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Formic acid, JIS special grade, ≥98.0%
Sigma-Aldrich
Acetic acid, SAJ first grade, ≥99.0%
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Acetic acid, 99.5-100.0%
Sigma-Aldrich
Acetic acid solution, 1 N, 1 M
Sigma-Aldrich
Acetic acid, ≥99.7%, suitable for amino acid analysis
Sigma-Aldrich
Acetic acid, JIS special grade, ≥99.7%
Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Acetic acid, suitable for luminescence, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Methanol, JIS special grade, ≥99.8%
Sigma-Aldrich
Methanol, SAJ special grade
Sigma-Aldrich
Methanol, SAJ first grade, ≥99.5%
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Methanol, suitable for HPLC
Sigma-Aldrich
Methanol, JIS 300, ≥99.8%, suitable for residue analysis
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, 99.93%