1H核磁共振法测定环境和生物样品中的β-N-甲基氨基-L-丙氨酸（L-BMAA）
1H NMR determination of beta-N-methylamino-L-alanine (L-BMAA) in environmental and biological samples.
作者信息
Moura Sidnei, Ultramari Mariah de Almeida, de Paula Daniela Mendes Louzada, Yonamine Mauricio, Pinto Ernani
机构信息
Departamento de Análises Clínicas e Toxicológicas, Faculdade de Ciências Farmacêuticas, Universidade de São Paulo, USP, Av. Professor Lineu Prestes, 580 813B CEP: 05508-900 São Paulo, SP, Brazil.
出版信息
Toxicon. 2009 Apr;53(5):578-83. doi: 10.1016/j.toxicon.2008.12.013.
A nuclear magnetic resonance (1H NMR) method for the determination of beta-N-methylamino-L-alanine (L-BMAA) in environmental aqueous samples was developed and validated. L-BMAA is a neurotoxic modified amino acid that can be produced by cyanobacteria in aqueous environments. This toxin was extracted from samples by means of solid-phase extraction (SPE) and identified and quantified by 1H NMR without further derivatization steps. The lower limit of quantification (LLOQ) was 5 microg/mL. Good inter and intra-assay precision was also observed (relative standard deviation <8.5%) with the use of 4-nitro-DL-phenylalanine as an internal standard (IS). This method of 1H NMR analysis is not time consuming and can be readily utilized to monitor L-BMAA and confirm its presence in environmental and biological samples.
开发并验证了一种用于测定环境水样中β-N-甲基氨基-L-丙氨酸（L-BMAA）的核磁共振（1H NMR）方法。L-BMAA是一种神经毒性修饰氨基酸，可由水环境中的蓝细菌产生。该毒素通过固相萃取（SPE）从样品中提取，无需进一步衍生步骤，即可通过1H NMR进行鉴定和定量。定量下限（LLOQ）为5微克/毫升。使用4-硝基-DL-苯丙氨酸作为内标（IS）时，还观察到了良好的批间和批内精密度（相对标准偏差<8.5%）。这种1H NMR分析方法不耗时，可轻松用于监测L-BMAA并确认其在环境和生物样品中的存在。
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