On-line solid-phase extraction coupled to liquid chromatography tandem mass spectrometry for the analysis of cyanotoxins in algal blooms.
An analytical method based on on-line SPE-LC-HESI-MS/MS has been developed for the detection and quantification of eight selected cyanotoxins in algal bloom waters that include mycrocystins, anatoxin-a and cylindrospermopsin. The injection volume was 2 mL according to the expected concentration of cyanotoxins in matrix. The method provides an analysis time of 7 min per sample, acceptable recovery values (91-101%), good precision (RSD < 13%) and method limits of detection at the sub-microgram per liter levels (0.01-0.02 μg L(-1)). A detailed discussion on optimization parameters that have an impact on the overall performance of the method are presented. In particular, method optimization permitted the chromatographic separation of anatoxin-a and phenylalanine, an isobaric interference with a similar chromatographic characteristics. All optimization and validation experiments for the on-line SPE method and chromatographic separation were performed in environmentally relevant algal bloom water matrices. The applicability of the method was tested on several algal bloom water samples from monitored lakes across the province of Québec (Québec, Canada) known to produce cyanotoxins. All of the targeted cyanotoxins were detected with the exception of cylindrospermopsin. In addition, it was found that total microcystin concentrations in several surface water samples exceeded the proposed guidelines established by the province of Québec in Canada of 1.5 μg L(-1) as well as the World Health Organization of 1 μg L(-1) for both free and cell-bound microcystin-LR equivalent.
Department of Chemistry, Université de Montréal, Montreal, QC, Canada.
Paul B
PB
Fayad
Department of Chemistry, Université de Montréal, Montreal, QC, Canada.
Audrey
A
Roy-Lachapelle
Department of Chemistry, Université de Montréal, Montreal, QC, Canada.
Sung Vo
SV
Duy
Department of Civil, Geological and Mining Engineering, Polytechnique Montréal, Montreal, QC, Canada.
Michèle
M
Prévost
Department of Chemistry, Université de Montréal, Montreal, QC, Canada. Electronic address: sebastien.sauve@umontreal.ca.
Sébastien
S
Sauvé
D000470:Alkaloids; D001427:Bacterial Toxins / Q000032:analysis / Q000737:chemistry*; D002853:Chromatography, Liquid; D000458:Cyanobacteria / Q000737:chemistry*; D000087522:Cyanobacteria Toxins; D004784:Environmental Monitoring / Q000379:methods*; D057097:Harmful Algal Bloom; D008387:Marine Toxins / Q000032:analysis / Q000737:chemistry*; D052998:Microcystins / Q000032:analysis / Q000737:chemistry; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry; D014326:Tropanes / Q000032:analysis / Q000737:chemistry; D014498:Uracil / Q000031:analogs & derivatives / Q000032:analysis / Q000737:chemistry
D000470:Alkaloids; D001427:Bacterial Toxins; D000087522:Cyanobacteria Toxins; D008387:Marine Toxins; D052998:Microcystins; D014326:Tropanes; C089595:cylindrospermopsin; D014498:Uracil; C078588:microcystin; C509783:anatoxin a
ANA-a; Anatoxin; Bleu green algae; Cyanotoxins; Mass spectrometry; Microcystin; Online SPE