title: Ultra-trace levels analysis of microcystins and nodularin in surface water by on-line solid-phase extraction with high-performance liquid chromatography tandem mass spectrometry.
abstract: An on-line solid phase extraction coupled with high-performance liquid chromatography in tandem with mass spectrometry (on-line SPE/HPLC/MS-MS) method for the determination of five microcystins and nodularin in surface waters at submicrogram per liter concentrations has been optimized. Maximum recoveries were achieved by carefully optimizing the extraction sample volume, loading solvent, wash solvent, and pH of the sample. The developed method was also validated according to both UNI EN ISO IEC 17025 and UNICHIM guidelines. Specifically, ten analytical runs were performed at three different concentration levels using a reference mix solution containing the six analytes. The method was applied for monitoring the concentrations of microcystins and nodularin in real surface water during a sampling campaign of 9 months in which the ELISA method was used as standard official method. The results of the two methods were compared showing good agreement when the highest concentration values of MCs were found. Graphical abstract An on-line SPE/HPLC/MS-MS method for the determination of five microcystins and nodularin in surface waters at sub μg L(-1) was optimized and compared with ELISA assay method for real samples.
authors.affiliation: Acquedotto Pugliese S.p.A., Area Controllo Qualità, Direzione Operativa (DOPRI), Viale Emanuele Orlando, Bari, 70121, Italy.
authors.forename: Lydia
authors.initials: L
authors.lastname: Balest
authors.affiliation: Consiglio Nazionale delle Ricerche, Istituto di Ricerca Sulle Acque, Viale F. De Blasio 5, Bari, 70132, Italy.
authors.forename: Sapia
authors.initials: S
authors.lastname: Murgolo
authors.affiliation: Acquedotto Pugliese S.p.A., Area Controllo Qualità, Direzione Operativa (DOPRI), Viale Emanuele Orlando, Bari, 70121, Italy.
authors.forename: Lucia
authors.initials: L
authors.lastname: Sciancalepore
authors.affiliation: Acquedotto Pugliese S.p.A., Area Controllo Qualità, Direzione Operativa (DOPRI), Viale Emanuele Orlando, Bari, 70121, Italy.
authors.forename: Patrizia
authors.initials: P
authors.lastname: Montemurro
authors.affiliation: Acquedotto Pugliese S.p.A., Area Controllo Qualità, Direzione Operativa (DOPRI), Viale Emanuele Orlando, Bari, 70121, Italy.
authors.forename: Pier Paolo
authors.initials: PP
authors.lastname: Abis
authors.affiliation: Consiglio Nazionale delle Ricerche, Istituto di Ricerca Sulle Acque, Viale F. De Blasio 5, Bari, 70132, Italy.
authors.forename: Carlo
authors.initials: C
authors.lastname: Pastore
authors.affiliation: Consiglio Nazionale delle Ricerche, Istituto di Ricerca Sulle Acque, Viale F. De Blasio 5, Bari, 70132, Italy. giuseppe.mascolo@ba.irsa.cnr.it.
authors.forename: Giuseppe
authors.initials: G
authors.lastname: Mascolo
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004784:Environmental Monitoring; D052998:Microcystins / Q000737:chemistry* / Q000302:isolation & purification*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000737:chemistry* / Q000302:isolation & purification*
chemical_list: D052998:Microcystins; D014874:Water Pollutants, Chemical; C078588:microcystin
keywords: Demethylated microcystins; Microcystins; On-line SPE/HPLC/MS-MS