Quantitative analysis of tetramethylenedisulfotetramine (tetramine) spiked into beverages by liquid chromatography-tandem mass spectrometry with validation by gas chromatography-mass spectrometry.
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.
Forensic Science Center, L-091, Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, California 94550, USA. owens33@llnl.gov
Janel
J
Owens
Saphon
S
Hok
Armando
A
Alcaraz
Carolyn
C
Koester
D000818:Animals; D001628:Beverages / Q000032:analysis*; D001952:Bridged-Ring Compounds / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D005638:Fruit; D008401:Gas Chromatography-Mass Spectrometry; D008892:Milk / Q000737:chemistry; D015203:Reproducibility of Results; D012378:Rodenticides / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013662:Tea / Q000737:chemistry; D014867:Water / Q000737:chemistry
D001952:Bridged-Ring Compounds; D012378:Rodenticides; D013662:Tea; D014867:Water; C010349:tetramethylenedisulfotetramine