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

被引:23
作者
Balest, Lydia [1 ]
Murgolo, Sapia [2 ]
Sciancalepore, Lucia [1 ]
Montemurro, Patrizia [1 ]
Abis, Pier Paolo [1 ]
Pastore, Carlo [2 ]
Mascolo, Giuseppe [2 ]
机构
[1] Acquedotto Pugliese SpA, Area Controllo Qualita, Direz Operat DOPRI, Viale Emanuele Orlando, I-70121 Bari, Italy
[2] CNR, Ist Ric Acque, Viale F De Blasio 5, I-70132 Bari, Italy
关键词
Microcystins; Demethylated microcystins; On-line SPE/HPLC/MS-MS; CYANOBACTERIA; HEPATOTOXINS;
D O I
10.1007/s00216-016-9495-y
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
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.
引用
收藏
页码:4063 / 4071
页数:9
相关论文
共 21 条
[1]   A heuristic derivation of the Horwitz curve [J].
Albert, R ;
Horwitz, W .
ANALYTICAL CHEMISTRY, 1997, 69 (04) :789-790
[2]   Determination of six microcystins and nodularin in surface and drinking waters by on-line solid phase extraction-ultra high pressure liquid chromatography tandem mass spectrometry [J].
Beltran, Eduardo ;
Ibanez, Maria ;
Vicente Sancho, Juan ;
Hernandez, Felix .
JOURNAL OF CHROMATOGRAPHY A, 2012, 1266 :61-68
[3]  
Carmichael WW, 1999, NAT TOXINS, V7, P377, DOI 10.1002/1522-7189(199911/12)7:6<377::AID-NT80>3.0.CO
[4]  
2-8
[5]   Seasonal occurrence and toxicity of Micyocystis spp. and.7 Oscillatoria tenuis in the Lebna Dam, Tunisia [J].
El Herry, Soumaya ;
Fathalli, Afef ;
Rejeb, Amel Jenhani-Ben ;
Bouaicha, Noureddine .
WATER RESEARCH, 2008, 42 (4-5) :1263-1273
[6]  
Hrudey S., 1994, Toxic Cyanobacteria - A Global Perspective, P7
[7]  
Kozacek C, 2014, GREAT LAKES MAYORS A
[8]   Evaluation of methods for the isolation, detection and quantification of cyanobacterial hepatotoxins [J].
Msagati, Titus A. M. ;
Siame, Bupe A. ;
Shushu, Deborah D. .
AQUATIC TOXICOLOGY, 2006, 78 (04) :382-397
[9]   Detection of various freshwater cyanobacterial toxins using ultra-performance liquid chromatography tandem mass spectrometry [J].
Oehrle, Stuart A. ;
Southwell, Ben ;
Westrick, Judy .
TOXICON, 2010, 55 (05) :965-972
[10]   Recent advances in the sample preparation, liquid chromatography tandem mass spectrometric analysis and environmental fate of microcystins in water [J].
Pérez, S ;
Aga, DS .
TRAC-TRENDS IN ANALYTICAL CHEMISTRY, 2005, 24 (07) :658-670