FOOD SCIENCE ›› 2013, Vol. 34 ›› Issue (2): 170-174.

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Analysis of gonyautoxins (GTXs) by a post-column derivatization high performance liquid chromatography

  

  • Received:2011-11-12 Revised:2012-12-20 Online:2013-01-25 Published:2013-01-15
  • Contact: Hua-Juan LIN E-mail:huajuanlin@vip.163.com

Abstract:

Paralytic shellfish poisoning (PSP) toxins is an important risk for sea food safety, and detecting technology of high performance liquid chromatography (HPLC) for PSP toxins is an important part for promoting safety supervision system of sea food in China. In this paper, effects of post-column derivatization condition on reaction fluorescent intensity and mobile phase condition on separation of gonyautoxins (GTXs) base on HPLC were discussed. Analysis of post-column derivatization showed the effects of pH of reaction solution, reaction temperature, formamide concentration and ammonium formate concentration on fluorescent sensitivity of individual GTX compounds were remarkable different. Considering the relationship between reaction fluorescent intensity and reaction conditions, the optimum post-column derivatization conditions were defined as: reaction solution mixtured by 70 mmol/L periodic acid and 0.12 mol/L potassium hydrate, 0.75 mol/L formamide of 20% ammonium formate solution, with pH of 7.3~7.5, flow rate of 0.8 ml/min, and reaction temperature of 50℃. Analysis of mobile phase showed the effects of methanol concentration, sodium heptanesulfonate concentration, pH, and phosphate concentration on separation of GTXs were all obvious, and the optimum mobile phase conditions were determined as: the concentrations of methanol, sodium heptanesulfonate, phosphate were 1%, 1.5 mmol/L, 10 mmol/L respectively, with pH of 7.3. Comparison to HPLC of oshima method, the response rate of GTX1, GTX3 and GTX4 increased to 4.7, 3.4 and 3.8 times, respectively, beside that of GTX2.

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