PMID- 23107121
OWN - NLM
STAT- MEDLINE
DCOM- 20130219
LR  - 20161125
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1266
DP  - 2012 Nov 30
TI  - 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.
PG  - 61-8
LID - S0021-9673(12)01572-5 [pii]
LID - 10.1016/j.chroma.2012.10.017 [doi]
AB  - Microcystins and nodularin are cyclic peptides hepatotoxins produced by 
      cyanobacterial genera (blue-green algae). Toxic cyanobacterial blooms are a 
      worldwide problem, as reported in several countries, like China, Australia, or 
      the United States. Therefore, it is necessary to develop sensitive and reliable 
      analytical methodology to determine this type of toxins in water at parts per 
      billion levels, or even lower. In this work, the potential of solid-phase 
      extraction coupled on-line to ultra-high-pressure liquid 
      chromatography/electrospray tandem mass spectrometry (SPE-UHPLC-MS/MS) has been 
      investigated for the efficient quantification and confirmation of microcystins 
      LR, RR, YR, LY, LW, LF and nodularin in surface and drinking water samples, at 
      sub-ppb levels. The method developed involves the injection of only 1 mL of water 
      sample into the on-line SPE-UHPLC-MS/MS system and allows the rapid determination 
      of the compounds selected (8 min of chromatographic run), avoiding laborious 
      sample treatment. The method was validated in surface and drinking water by means 
      of recovery experiments at 0.25 and 1 mug L(-1). Average recoveries (n=5) ranged 
      from 71 to 116%, with relative standard deviations (RSDs) lower than 15%. For 
      microcystins LR, RR, YR and nodularin, a third level was also assayed (0.1 mug 
      L(-1)) obtaining satisfactory data too. Limits of detection between 0.002 and 
      0.0405 mug L(-1) were estimated (0.0005 mug L(-1) for nodularin). The developed 
      method was applied to the analysis of water samples collected in the province of 
      Castellon (Spain). The acquisition of three MS/MS transitions for each compound 
      allowed the unequivocal confirmation of positive samples, which was supported by 
      the accomplishment of ion intensity ratios and retention time when compared with 
      reference standards.
CI  - Copyright (c) 2012 Elsevier B.V. All rights reserved.
FAU - Beltran, Eduardo
AU  - Beltran E
AD  - Research Institute for Pesticides and Water, University Jaume I, E-12071 
      Castellon, Spain.
FAU - Ibanez, Maria
AU  - Ibanez M
FAU - Sancho, Juan Vicente
AU  - Sancho JV
FAU - Hernandez, Felix
AU  - Hernandez F
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20121016
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Drinking Water)
RN  - 0 (Microcystins)
RN  - 0 (Peptides, Cyclic)
RN  - 0 (Water Pollutants, Chemical)
RN  - 0979BIK2QU (nodularin)
SB  - IM
MH  - Chromatography, High Pressure Liquid/*methods
MH  - Drinking Water/*chemistry
MH  - Lakes/*chemistry
MH  - Limit of Detection
MH  - Microcystins/*analysis/chemistry/isolation & purification
MH  - Peptides, Cyclic/*analysis/chemistry/isolation & purification
MH  - Reproducibility of Results
MH  - Solid Phase Extraction/*methods
MH  - Tandem Mass Spectrometry/methods
MH  - Water Pollutants, Chemical/*analysis/chemistry/isolation & purification
EDAT- 2012/10/31 06:00
MHDA- 2013/02/21 06:00
CRDT- 2012/10/31 06:00
PHST- 2012/08/01 00:00 [received]
PHST- 2012/09/27 00:00 [revised]
PHST- 2012/10/08 00:00 [accepted]
PHST- 2012/10/31 06:00 [entrez]
PHST- 2012/10/31 06:00 [pubmed]
PHST- 2013/02/21 06:00 [medline]
AID - S0021-9673(12)01572-5 [pii]
AID - 10.1016/j.chroma.2012.10.017 [doi]
PST - ppublish
SO  - J Chromatogr A. 2012 Nov 30;1266:61-8. doi: 10.1016/j.chroma.2012.10.017. Epub 
      2012 Oct 16.