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Merck
  • Improvement on sample clean-up for high-performance liquid chromatographic-fluorimetric determination of diarrhetic shellfish toxins using 1-bromoacetylpyrene.

Improvement on sample clean-up for high-performance liquid chromatographic-fluorimetric determination of diarrhetic shellfish toxins using 1-bromoacetylpyrene.

Journal of chromatography. A (1998-02-20)
J C González, M R Vieytes, J M Vieites, L M Botana
要旨

Okadaic acid (OA) and dinophysistoxin-2, two of the main diarrhetic shellfish toxins, can be determined by high-performance liquid chromatography coupled to fluorimetry as pyrenacyl esters. Toxin fluorescent derivatives were obtained after quantitative derivatization with 1-bromoacetylpyrene in acetonitrile. An efficient improvement in the silica gel clean-up procedure of the pyrenacyl derivatives is reported. The clean-up cartridge is washed with hexane-dichloromethane (1:1, v/v), dichloromethane-ethyl acetate (8:2, v/v), and finally the pyrenacyl esters were eluted with dichloromethane-methanol (9:1, v/v). We compare this procedure with other methods already described. Good results were obtained with mussels, scallops and clams. The clean-up procedure showed good robustness when checked against silica and solvents activity. Using samples of mussel hepatopancreas with an OA concentration ranging from 0 to 2 micrograms OA/g hepatopancreas, the inter-assay relative standard deviation ranged from 5.5 to 12.6%.

材料
製品番号
ブランド
製品内容

Sigma-Aldrich
1-(ブロモアセチル)ピレン, 97%