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Optimization of matrix solid-phase dispersion for the rapid determination of salicylate and benzophenone-type UV absorbing substances in marketed fish

Authors
Journal
Food Chemistry
0308-8146
Publisher
Elsevier
Publication Date
Volume
154
Identifiers
DOI: 10.1016/j.foodchem.2014.01.013
Keywords
  • Organic Uv Absorbing Substances
  • On-Line Silylation
  • Matrix Solid-Phase Dispersion
  • Gc–Ms/Ms
  • Fish Sample Analysis
Disciplines
  • Design

Abstract

Abstract A simple and effective method for the rapid determination of five salicylate and benzophenone-type UV absorbing substances in marketed fish is described. The method involves the use of matrix solid-phase dispersion (MSPD) prior to their determination by on-line silylation gas chromatography tandem mass spectrometry (GC–MS/MS). The parameters that affect the extraction efficiency were optimized using a Box–Behnken design method. The optimal extraction conditions involved dispersing 0.5g of freeze-dried powdered fish with 1.0g of Florisil using a mortar and pestle. This blend was then transferred to a solid-phase extraction (SPE) cartridge containing 1.0g of octadecyl bonded silica (C18), as the clean-up co-sorbent. The target analytes were then eluted with 7mL of acetonitrile. The extract was derivatized on-line in the GC injection-port by reaction with a trimethylsilylating (TMS) reagent. The TMS-derivatives were then identified and quantitated by GC–MS/MS. The limits of quantitation (LOQs) were less than 0.1ng/g.

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