Total Analysis of Microcystins in Fish Tissue Using Laser Thermal Desorption鈥揂tmospheric Pressure Chemical Ionization鈥揌igh-Resolution Mass Spectrometry (LDTD-APCI-HRMS)

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• 作者：Audrey Roy-Lachapelle ; Morgan Solliec ; Marc Sinotte ; Christian Deblois ; S茅bastien Sauv茅
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2015
• 出版时间：August 26, 2015
• 年：2015
• 卷：63
• 期：33
• 页码：7440-7449
• 全文大小：400K
• ISSN：1520-5118

文摘

Microcystins (MCs) are cyanobacterial toxins encountered in aquatic environments worldwide. Over 100 MC variants have been identified and have the capacity to covalently bind to animal tissue. This study presents a new approach for cell-bound and free microcystin analysis in fish tissue using sodium hydroxide as a digestion agent and Lemieux oxidation to obtain the 2-methyl-3-methoxy-4-phenylbutyric acid (MMPB) moiety, common to all microcystin congeners. The use of laser diode thermal desorption鈥揳tmospheric pressure chemical ionization coupled with Q-Exactive mass spectrometry (LDTD-APCI-HRMS) led to an analysis time of approximately 10 s per sample and high-resolution detection. Digestion/oxidation and solid phase extraction recoveries ranged from 70 to 75% and from 86 to 103%, respectively. Method detection and quantification limits values were 2.7 and 8.2 渭g kg^鈥?, respectively. Fish samples from cyanobacteria-contaminated lakes were analyzed, and concentrations ranging from 2.9 to 13.2 渭g kg^鈥? were reported.