Carter Jake A, Barber Charles A, Wolle Mesay M, Gray Patrick J
Human Foods Program, Office of Laboratory Operations & Applied Science, US Food & Drug Administration, 5001 Campus Drive, College Park, MD, 20740, USA.
Anal Bioanal Chem. 2025 Aug;417(20):4723-4738. doi: 10.1007/s00216-025-05989-8. Epub 2025 Jul 16.
Accurate technologies and methods are needed to monitor both total and methylmercury in the marine food supply. Thermal decomposition gold amalgamation atomic absorption spectrophotometry (TDA-AAS) is an efficient and cost-effective technique for measuring low levels of total mercury requiring no sample preparation. Measuring methylmercury with TDA-AAS requires isolating methylmercury from the matrix and other mercury species prior to detection. We developed a method that uses ethyl acetate instead of a legacy non-polar solvent, toluene. Toluene is a potentially hazardous and problematic solvent whereas ethyl acetate is greener and safer. Additionally, the salting-out assisted liquid-liquid extraction (SALLE) approach with ethyl acetate avoids emulsion formation throughout extraction. We describe method development and validation of a SALLE and TDA-AAS detection for methylmercury in finfish. From 10 reference materials, our method recovered 80-118% of total or methylmercury with Z scores ranging from -1.98 to 2.75 (n = 184). The LOD and LOQ of the method for methylmercury were 3.8 and 27 ng/g, respectively. From extraction to detection, accurate results were obtained from a sample in less than 2 h for both total mercury and methylmercury.
需要精确的技术和方法来监测海洋食物供应中的总汞和甲基汞。热分解金汞齐化原子吸收分光光度法(TDA-AAS)是一种高效且经济的技术,用于测量低水平的总汞,无需样品制备。用TDA-AAS测量甲基汞需要在检测前从基质和其他汞物种中分离出甲基汞。我们开发了一种方法,使用乙酸乙酯代替传统的非极性溶剂甲苯。甲苯是一种潜在危险且有问题的溶剂,而乙酸乙酯更环保、更安全。此外,用乙酸乙酯进行盐析辅助液液萃取(SALLE)方法可避免整个萃取过程中形成乳液。我们描述了用于鱼类中甲基汞的SALLE和TDA-AAS检测的方法开发和验证。从10种参考物质中,我们的方法回收了80%-118%的总汞或甲基汞,Z分数范围为-1.98至2.75(n = 184)。该方法对甲基汞的检测限和定量限分别为3.8和27 ng/g。从萃取到检测,总汞和甲基汞的样品在不到2小时内即可获得准确结果。