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Cylindrospermopsin determination using 2-[4-(2-hydroxyethyl)-1-piperazinyl]ethanesulfonic acid (HEPES) as the internal standard
Authors:Kikuchi Sachiko  Kubo Takuya  Kaya Kunimitsu
Affiliation:Graduate School of Environmental Studies, Tohoku University, 6-6-20, Aoba, Aramaki, Aoba-ku, Sendai 980-8579, Japan
Abstract:Cylindrospermopsin (CYN) was determined by liquid chromatography/electrospray ionization-mass spectrometry (LC/ESI-MS) using 2-[4-(2-hydroxyethyl)-1-piperazinyl]ethanesulfonic acid (HEPES) as the internal standard. In the selected ion monitoring of LC/ESI-MS, m/z 414 for CYN and 237 for HEPES were monitored using the negative mode; the retention times of CYN and HEPES were 12.41 and 14.21 min, respectively. CYN was determined from peak area ratios of m/z 414/237. By the treatment of an anion exchange cartridge using a buffer at pH 10.5, CYN was isolated and condensed. No interfering peak was observed. Linearity of this method was observed at the range of 0.10-31.12 ng. Total coefficients of variation were 5.1 and 2.9% at 104 and 1038 μg CYN L−1. The quantitative limit at a signal-to-noise (S/N) ratio of 10 was 0.16 ng.CYN concentration in natural waters is low. CYN in waters should be condensed for determination. This method including the treatment for isolation and condensation of CYN is useful for determination of CYN in environmental and/or drinking waters.
Keywords:Cyanobacterial toxin   Cylindrospermopsin   Internal standard   (2[4-(2-Hydroxyethyl)-1-piperazinyl]ethanesulfonic acid) (HEPES)   Liquid chromatography/electrospray ionization-mass spectrometry (LC/ESI-MS)   Selected ion monitoring (SIM)
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