Determination of yessotoxins and pectenotoxins in shellfish by capillary electrophoresis-electrospray ionization-mass spectrometry.
Conditions for the determination of lipophilic marine toxins, such as yessotoxins and pectenotoxins (PTX)-6, were investigated with capillary electrophoresis coupled to mass spectrometry (MS) with an electrospray ionization source. After optimization, a simple and MS compatible alkaline volatile buffer solution of ammonium acetate was selected as background electrolyte, with isopropanol/water (80/20, v/v) sheath liquid modified with ammonium acetate used at the electrospray ionization (ESI) source. Previously to capillary electrophoresis (CE) separations, the application of an on-line sample pre-concentration approach based on field-amplified sample stacking was accomplished to increase sensitivity. As a result, the limits of detection provided by capillary electrophoresis-electrospray ionization-mass spectrometry (CE-ESI-MS) were 0.02 microg ml(-1) (0.01 microg g(-1)), which corresponded to 1.25 pg for yessotoxin and 0.25 microg ml(-1) (0.13 microg g(-1) and 13.25 pg on capillary) for PTX-6. Accuracy tests showed 97.7% recovery from spiked blank mussel samples that showed no significant matrix influence running under optimal conditions. Intermediate precision was close to 4% relative standard deviation (RSD) for the migration time, and an RSD of 7.5% for peak areas. The method was successfully applied to naturally contaminated seafood samples in which yessotoxins and pectenotoxins-6 were clearly determined. This work demonstrated the potential of CE-ESI-MS to be applied for a sensitive determination of lipophilic toxins from the marine environment as alternative to liquid chromatography-electrospray ionization-single quadrupole mass spectrometry (LC-ESI-MS) for this purpose.
de la Iglesia
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Facultad de Química, Departamento de Química Analítica y Alimentaria, Universidad de Vigo, Vigo, Spain.
Gago-Martínez
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D000818:Animals; D005663:Furans / Q000032:analysis / Q000737:chemistry; D018942:Macrolides; D008387:Marine Toxins / Q000032:analysis* / Q000737:chemistry; D008978:Mollusk Venoms; D035964:Oxocins / Q000032:analysis* / Q000737:chemistry; D011714:Pyrans / Q000032:analysis / Q000737:chemistry; D012680:Sensitivity and Specificity; D012758:Shellfish / Q000032:analysis*; D013030:Spain; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D000095702:Polyether Toxins
D005663:Furans; D018942:Macrolides; D008387:Marine Toxins; D008978:Mollusk Venoms; D035964:Oxocins; D011714:Pyrans; C114399:pectenotoxin 6; D000095702:Polyether Toxins; C051905:pectenotoxin 1; C098380:pectenotoxin 2; C066632:yessotoxin