Related Experiment Video For HILIC
Updated: Mar 20, 2026
Integration of Miniaturized Solid Phase Extraction and LC-MS/MS Detection of 3-Nitrotyrosine in Human Urine for Clinical Applications
Published on: July 14, 2017
Development and validation of a high-throughput online solid phase extraction - Liquid chromatography - Tandem mass
Rebecca Coleman1, Sharon W Lemire1, William Bragg1
1Division of Laboratory Sciences, National Centers for Environmental Health, Centers for Disease Control and Prevention, 4770 Buford Highway, MS F44, Atlanta, GA 30341, USA.
Abstract:
Tetrodotoxin (TTX) is an extremely potent paralytic toxin responsible for yearly illness and death around the world. A clinical measurement is necessary to confirm exposure because symptoms of TTX intoxication cannot be distinguished from other paralytic toxins. Our group has developed an online solid phase extraction hydrophilic interaction liquid chromatography (HILIC) method for the analysis of TTX in human urine with tandem mass spectrometry. The reportable range for the method was 2.80 - 249 ng/mL in urine with precision and accuracy within 15% as determined for all quality control samples. No isotopically-labeled internal standard is available for TTX; thus a surrogate internal standard, voglibose, was investigated to compensate for matrix effects and ionization suppression. However, upon evaluation, voglibose was ineffective for this purpose. This new online method rapidly identifies TTX, facilitating the work of public health authorities and providing support to monitoring programs worldwide.
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