Quantitative analysis of tetramethylenedisulfotetramine (tetramine) spiked into beverages by liquid chromatography-tandem mass spectrometry with validation by gas chromatography-mass spectrometry.

Abstract

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.

• Authors: Janel Owens, Saphon Hok, Armando Alcaraz, Carolyn Koester
• Journal: Journal of agricultural and food chemistry (J Agric Food Chem) Vol. 57 Issue 10 Pg. 4058-67 (May 27 2009) ISSN: 1520-5118 [Electronic] United States
• PMID: 19358574 (Publication Type: Journal Article, Research Support, U.S. Gov't, Non-P.H.S.)

Chemical References

• Bridged-Ring Compounds
• Rodenticides
• Tea
• Water
• tetramethylenedisulfotetramine

Topics

• Animals
• Beverages (analysis)
• Bridged-Ring Compounds (analysis)
• Chromatography, High Pressure Liquid (methods)
• Food Contamination (analysis)
• Fruit
• Gas Chromatography-Mass Spectrometry
• Milk (chemistry)
• Reproducibility of Results
• Rodenticides (analysis)
• Tandem Mass Spectrometry (methods)
• Tea (chemistry)
• Water (chemistry)