Liquid Chromatography-Tandem Mass Spectrometry Application, for the Determination of Extracellular Hepatotoxins in Irish Lake and Drinking Waters
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- 作者：Orla Allis ; Justine Dauphard ; Brett Hamilton ; Aine Ni Shuilleabhain ; Mary Lehane ; Kevin J. James ; Ambrose Furey
- 刊名：Analytical Chemistry
- 出版年：2007
- 出版时间：May 1, 2007
- 年：2007
- 卷：79
- 期：9
- 页码：3436 - 3447
- 全文大小：284K
- 年卷期：v.79,no.9(May 1, 2007)
- ISSN：1520-6882
文摘
A novel method for the determination of hepatotoxins;microcystins (MCs), and nodularin (Nod) in lake waterand domestic chlorinated tap water has been developedusing liquid chromatography hyphenated with electrospray ionization triple quadrupole mass spectrometry (LC-ESI-MS/MS). Optimization of the mass spectrometerparameters and mobile-phase composition was performedto maximize the sensitivity and reproducibility of themethod. Detection of the hepatotoxins was carried outusing multiple reaction monitoring experiments, thusimproving the selectivity of the method. A total ionchromatogram and a precursor ion scan on ion m/z 135was also applied to all samples to detect unknown microcystins or microcystins for which there are no standardsavailable. A comprehensive validation of the LC-ESI-MS/MS method was completed that took into account matrixeffects, specificity, linearity, accuracy, and precision.Good linear calibrations were obtained for MC-LR (1-200 
r.gif">g/L; R2 = 0.9994) in spiked lake and tap watersamples (1-50 r.gif">g/L; R2 = 0.9974). Acceptable interdayrepeatability was achieved for MC-LR in lake water withRSD values (n = 9) ranging from 9.9 (10 r.gif">g/L) to 5.1%(100 r.gif">g/L). Excellent limits of detection (LOD) and limitsof quantitation (LOQ) were achieved with spiked MCs andNod samples; LOD = 0.27 r.gif">g/L and LOQ = 0.90 r.gif">g/Lfor MC-LR in the "normal linear range" and LOD = 0.08r.gif">g/L and LOQ = 0.25 r.gif">g/L in the "low linear range" inboth lake and chlorinated tap water. Similar results wereobtained for a suite of microcystins and nodularin. Thissensitive and rapid method does not require any samplepreconcentration, including the elimination of solid-phaseextraction (SPE) for the effective screening of hepatotoxinsin water below the 1 r.gif">g/L WHO provisional guideline limitfor MC-LR. Furthermore, SPE techniques are time-consuming, nonreproducible at trace levels, and offerpoor recoveries with chlorinated water. The applicationof this LC-ESI-MS/MS method for routine screening ofhepatotoxins in lake and chlorinated tap water (averageCl2 = 0.23 mg/L) is achieved and this study representsthe first direct method for the screening of hepatotoxinsin chlorinated tap water.
r.gif">g/L; R2 = 0.9994) in spiked lake and tap watersamples (1-50 r.gif">g/L; R2 = 0.9974). Acceptable interdayrepeatability was achieved for MC-LR in lake water withRSD values (n = 9) ranging from 9.9 (10 r.gif">g/L) to 5.1%(100 r.gif">g/L). Excellent limits of detection (LOD) and limitsof quantitation (LOQ) were achieved with spiked MCs andNod samples; LOD = 0.27 r.gif">g/L and LOQ = 0.90 r.gif">g/Lfor MC-LR in the "normal linear range" and LOD = 0.08r.gif">g/L and LOQ = 0.25 r.gif">g/L in the "low linear range" inboth lake and chlorinated tap water. Similar results wereobtained for a suite of microcystins and nodularin. Thissensitive and rapid method does not require any samplepreconcentration, including the elimination of solid-phaseextraction (SPE) for the effective screening of hepatotoxinsin water below the 1 r.gif">g/L WHO provisional guideline limitfor MC-LR. Furthermore, SPE techniques are time-consuming, nonreproducible at trace levels, and offerpoor recoveries with chlorinated water. The applicationof this LC-ESI-MS/MS method for routine screening ofhepatotoxins in lake and chlorinated tap water (averageCl2 = 0.23 mg/L) is achieved and this study representsthe first direct method for the screening of hepatotoxinsin chlorinated tap water.