Forensic Science Center, L-091, Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, California 94550, USA.
J Agric Food Chem. 2009 May 27;57(10):4058-67. doi: 10.1021/jf900271z. Epub 2009 Apr 9.
Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD(50) = 0.1 mg/kg) used in hundreds of deliberate and accidental food poisoning events in China. This paper describes a method for the quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water, with cleanup by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography-mass spectrometry (GC-MS) operated in selected ion monitoring mode for ions m/z 212, 240, and 360. The limit of quantitation was 0.10 μg/mL by LC-MS/MS versus 0.15 μg/mL for GC-MS. Fortifications of the beverages at 2.5 and 0.25 μg/mL were recovered ranging from 73 to 128% by liquid-liquid extraction for GC-MS analysis, from 13 to 96% by SPE, and from 10 to 101% by liquid-liquid extraction for LC-MS/MS analysis.
四亚甲基二砜四胺，俗称毒鼠强，是一种高神经毒性的灭鼠剂（人体口服 LD(50) = 0.1 毫克/千克），在中国已被用于数百起因故意或意外而导致的食物中毒事件中。本文介绍了一种测定掺入饮料（包括牛奶、果汁、茶、可乐和水）中的毒鼠强的方法，包括 C8 固相萃取和液液萃取的净化过程。采用高效液相色谱-串联质谱法（LC-MS/MS），根据 m/z 347 到 m/z 268 的碎片进行定量。该方法通过气相色谱-质谱法（GC-MS），在选择离子监测模式下，对 m/z 212、240 和 360 的离子进行验证。LC-MS/MS 的定量下限为 0.10 μg/mL，而 GC-MS 的定量下限为 0.15 μg/mL。通过液液萃取对饮料进行 2.5 和 0.25 μg/mL 的添加，经 GC-MS 分析的回收率范围为 73%至 128%，经 SPE 的回收率范围为 13%至 96%，经 LC-MS/MS 分析的回收率范围为 10%至 101%。
