Journal
JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
Volume 63, Issue 12, Pages 3129-3134Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.jafc.5b00045
Keywords
tetrodotoxin; immunoaffinity; ultrahigh performance liquid chromatography tandem mass spectrometry
Funding
- National Natural Science Foundation of China [81470148]
- National Key Technology R&D Program during the 12th Five-Year Plan [2012BAD29B06]
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A highly selective and sensitive method was developed for the determination of tetrodotoxin (TTX) in marine organisms by immunoaffinity chromatography (IAC) purification coupled with ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). An IAC column was prepared and used to cleanup the extracted samples. The operating conditions of the IAC column were optimized, and the capacity of new IAC column was found to be 1106 ng mL(-1), which was sufficient for TTX determination. The MS/MS conditions and UPLC mobile phase were also studied to optimize the operation conditions. Fortified marine organism samples at levels of 0.3-5.0 ng g(-1) were utilized, and the average recoveries were 86.5-103.6% with intra- and inter-day relative standard deviations less than 7.22 and 9.88%, respectively. The limits of detection and quantification were 0.1 and 0.3 ng g(-1), respectively. The method was later successfully applied for the determination of TTX in 100 marine organism samples collected from local markets.
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