Development and validation of a high-throughput double solid phase extraction–liquid chromatography–tandem mass spectrometry method for the determination of tetrodotoxin in human urine and plasma

Fong, Bonnie Mei-Wah; Tam, Sidney; Tsui, Sik-Hon; Leung, Kelvin Sze-Yin

doi:10.1016/j.talanta.2010.11.014

Cited by 35 publications

(28 citation statements)

References 17 publications

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“…Fong et al ., 2011 [135] stated that acetonitrile and methanol give similar recoveries and in view of the global shortage of acetonitrile and consequently its increased expense the preferred choice must be methanol. The same group found that non-acidified solutions tend not to retain TTX so they used 2% acetic acid to enhance retention.…”

Section: Historical Perspective On Analytical Methods Used For Ttmentioning

confidence: 99%

“…Its structure was elucidated by R. B. Woodward in 1964 [133]. Authentic standards for TTX are available from various commercial sources (Table 2); Wako Chemicals (Purity >90%) [134], Latoxan (Valence, France) [43], Sigma Aldrich (St. Louis, MO, USA), 99% HPLC [104,135], Sankyo Co., Ltd, Tokyo, Japan [136], Calbiochem, EMD Millipore, USA, [51], Ascent Scientific [137] and Axxora, Grunberg, Germany [138]. …”

Section: Structures and Standards For Ttx And Its Analoguesmentioning

confidence: 99%

“…This is because urine TTX levels depend not only on the amount of TTX ingested but also on the hydration state of the victim. While analysing TTX in urine, it is necessary to do a creatinine adjustment in order to eliminate the effects of the variations in the urinary outputs between patients [135]. Zimmer, 2010 [97] found a strong correlation between blood TTX levels and the poisoning symptoms.…”

Section: Clinical Studymentioning

confidence: 99%

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Tetrodotoxin: Chemistry, Toxicity, Source, Distribution and Detection

Bane

Lehane

Dikshit

et al. 2014

Toxins

325

286

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Tetrodotoxin (TTX) is a naturally occurring toxin that has been responsible for human intoxications and fatalities. Its usual route of toxicity is via the ingestion of contaminated puffer fish which are a culinary delicacy, especially in Japan. TTX was believed to be confined to regions of South East Asia, but recent studies have demonstrated that the toxin has spread to regions in the Pacific and the Mediterranean. There is no known antidote to TTX which is a powerful sodium channel inhibitor. This review aims to collect pertinent information available to date on TTX and its analogues with a special emphasis on the structure, aetiology, distribution, effects and the analytical methods employed for its detection.

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Section: Historical Perspective On Analytical Methods Used For Ttmentioning

confidence: 99%

Section: Structures and Standards For Ttx And Its Analoguesmentioning

confidence: 99%

Section: Clinical Studymentioning

confidence: 99%

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Tetrodotoxin: Chemistry, Toxicity, Source, Distribution and Detection

Bane

Lehane

Dikshit

et al. 2014

Toxins

325

286

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“…The LOD was 15.6 nM (5.0 ng/mL). Fong et al [17] developed a method that combined double solid phase extraction (C18 and hydrophilic interaction liquid chromatography) and analyzed by LC-MS/MS. The LOD and LOQ were 0.13 and 2.5 ng/mL, respectively.…”

Section: Introductionmentioning

confidence: 99%

A Study of 11-[3H]-Tetrodotoxin Absorption, Distribution, Metabolism and Excretion (ADME) in Adult Sprague-Dawley Rats

et al. 2017

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Tetrodotoxin (TTX) is a powerful sodium channel blocker that in low doses can safely relieve severe pain. Studying the absorption, distribution, metabolism and excretion (ADME) of TTX is challenging given the extremely low lethal dose. We conducted radiolabeled ADME studies in Sprague-Dawley rats. After a single dose of 6 µg/(16 µCi/kg) 11-[ 3 H]TTX, pharmacokinetics of plasma total radioactivity were similar in male and female rats. Maximum radioactivity (5.56 ng Eq./mL) was reached in 10 min. [ 3 H]TTX was below detection in plasma after 24 h. The area under the curve from 0 to 8 h was 5.89 h·ng Eq./mL; mean residence time was 1.62 h and t 1 2 was 2.31 h. Bile secretion accounted for 0.43% and approximately 51% of the dose was recovered in the urine, the predominant route of elimination. Approximately 69% was recovered, suggesting that hydrogen tritium exchange in rats produced tritiated water excreted in breath and saliva. Average total radioactivity in the stomach, lungs, kidney and intestines was higher than plasma concentrations. Metabolite analysis of plasma, urine and feces samples demonstrated oxidized TTX, the only identified metabolite. In conclusion, TTX was rapidly absorbed and excreted in rats, a standard preclinical model used to guide the design of clinical trials.

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“…They have been determined by HPLC with a post-column reaction and fluorescence detection or by HPLC with ultraviolet detection (Yasumoto and Tooru 1985;Yotsu et al 1989;Chen and Chou 1998;O'Leary, Schneider, and Isbister 2004;Jen et al 2008;Yu et al 2010). Alternatively, liquid chromatography-tandem mass spectrometry using ammonium heptafluorobutyrate as the ion-pair reagent has been reported (Shoji et al 2001;Akaki and Hatano 2006;Jang and Yotsu-Yamashita 2006;Jen et al 2008;Fong et al 2011;Leung, Fong, and Tsoi 2011). Ion-exchange chromatography mass spectrometry (MS) (Horie et al 2002;Hayashida et al 2004) and hydrophilic ion interaction chromatography tandem mass spectrometry (Jang and YotsuYamashita 2006;Nakagawa, Jang, and Yotsu-Yamashita 2006;Jen et al 2008;Jang, Lee, and Yotsu-Yamashita 2010;Leung, Fong, and Tsoi 2011) have also been used.…”

Section: Introductionmentioning

confidence: 99%

Evaluation of Helically Coiled and Knitted Open Tubular Reactors for the Efficient Post-Column Determination of Tetrodotoxin by High-Performance Liquid Chromatography

et al. 2016

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A post-column fluorescence reaction system for the high-performance liquid chromatographic (HPLC) determination of tetrodotoxin in the silver-cheeked toadfish Lagocephalus sceleratus is discussed theoretically and investigated experimentally. Ion-pair chromatography with volatile ammonium perfluoroheptanoate was used for the separation of tetrodotoxin and 4, 9-anhydrotetrodotoxin. The post-column reaction was based on tetrodotoxin conversion to a quinazoline fluorescent compound in strong alkaline conditions. All post-column parameters were optimized that affected the sensitivity, dispersion, and stability. Helically coiled and knitted open tubular reactors composed of polyetheretherketone were constructed and characterized in detail. The performance of these reactors was evaluated on the bases of sensitivity and dispersion. Their optimal design is reported. The knitted reactors were more efficient than the relevant helically coiled reactors when higher reaction times are required. A 1,500 μL polyetheretherketone knitted coil with 0.010″ internal diameter was optimum exhibiting higher pressure tolerances than Teflon coils. The HPLC post-column reaction method was evaluated in Downloaded by [University of Arizona] at 09:01 08 June 20163 terms of linearity, sensitivity, accuracy, precision, and ruggedness. The linear dynamic ranges for tetrodotoxin and 4, 9-anhydrotetrodotoxin were 40 to 3,000 ppb and 80 to 3,000 ppb, respectively. The limits of detection and quantification were 12 and 41 ppb for tetrodotoxin and 26 and 85 ppb for 4, 9-anhydrotetrodotoxin. The accuracy was evaluated by recovery measurements and the values for tetrodotoxin were between 90.7% and 93.6%. The use of a volatile perfuorocarboxylic acid as an ion-pair reagent allowed confirmation of by highperformance liquid chromatography -tandem mass spectrometry using identical mobile phase conditions.

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Development and validation of a high-throughput double solid phase extraction–liquid chromatography–tandem mass spectrometry method for the determination of tetrodotoxin in human urine and plasma

Cited by 35 publications

References 17 publications

Tetrodotoxin: Chemistry, Toxicity, Source, Distribution and Detection

Tetrodotoxin: Chemistry, Toxicity, Source, Distribution and Detection

A Study of 11-[3H]-Tetrodotoxin Absorption, Distribution, Metabolism and Excretion (ADME) in Adult Sprague-Dawley Rats

Evaluation of Helically Coiled and Knitted Open Tubular Reactors for the Efficient Post-Column Determination of Tetrodotoxin by High-Performance Liquid Chromatography

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