172 / 302
Table 2. Peak area precision (from five replicate injections) for
LC-MS/MS assay of MC-RR, MC-YR and MC-LR
Levels µg/L
MC-RR
MC-YR
MC-LR
0.05
16.01
10.5
6.91
0.10
2.82
5.88
3.97
0.20
3.54
5.25
4.89
0.50
4.86
8.54
3.03
1.00
5.84
1.76
4.25
5.00
2.28
2.13
2.47
10.00
4.54
1.30
1.31
50.00
2.40
1.76
2.66
Conclusion
A simple, sensitive and robust LC-MS method for
quantitative determination of microcystins was developed.
Targeted full-scan MS/MS analysis using the LTQ Velos
Pro linear ion trap mass spectrometer provided excellent
selectivity and sensitivity for the identification and
quantitation of MC-RR, MC-YR and MC-LR across a
wide linear dynamic range. The LOD and LOQ were
0.025 µg/L and 0.05 µg/L, respectively. The LOQ was
significantly lower than the provisional guideline value
established by the WHO for MC-LR concentrations in
drinking water. Assays performed in full-scan MS/MS
mode enable compound confirmation and quantitation
without the need for compound-dependent parameter
optimization. The method was used to analyze tap, filtered
and surface pond water. No microcystins were detected
from these three water sources.
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References
1.
Toxic cyanobacteria in water: A guide to their public
health consequences, monitoring and management;
Chorus I, Bartram J, eds. Published by E & FN Spon,
London, on behalf of the World Health Organization,
Geneva. 1999
2. Ingested Nitrate and Nitrite and Cyanobacterial Peptide
Toxins.
IARC Monogr Eval Carcinog Risks Hum,
2010
, 94:1–477.
3.
WHO Guidelines for Drinking-water Quality
, 3rd Ed.,
Vol. 1, Recommendations; WHO, Geneva. 2004
4.
ISO Water Quality: Determination of microcystins -
method using solid phase extraction (SPE) and high
performance liquid chromatography (HPLC) with
ultraviolet (UV) detection.
ISO, Geneva, Switzerland
(ISO 20179:2005).