作　　者： ; ; ; ; (秦小明）; (卢虹玉）;

机构地区： 广东海洋大学食品科技学院

出　　处： 《食品科学》 2013年第2期170-174,共5页

摘　　要： 探讨柱后衍生条件和流动相条件对膝沟藻毒素群(GTXs,麻痹性贝毒的一类)的反应荧光强度和分离效果的影响。柱后衍生条件分析结果显示,各GTXs对反应液pH值、温度、甲酰胺体积分数以及甲酸铵浓度等柱后衍生反应条件的感度有较大差异。确定最佳柱后衍生反应条件为70mmol/L高碘酸与含0.12mol/L氢氧化钾和0.75mol/L甲酸铵的20%甲酰胺溶液的混合液作为柱后衍生反应液、pH7.3～7.5、流速0.8min/mL、柱后反应温度50C。流动相条件分析结果显示,甲醇体积分数、庚烷磺酸钠浓度、pH值和磷酸浓度均显著影响各GTXs的保留时间和分离效果,确定最佳流动相条件为甲醇体积分数1%、庚烷磺酸钠浓度1.5mmol/L、磷酸浓度10mmol/L、pH7.3。灵敏度分析结果显示,除GTX2无明显差异外,GTX1、GTX3和GTX4的灵敏度分别为大岛法的4.7、3.4、3.8倍。 In this study, the effect of post-column derivatization conditions on fluorescent intensity of reaction products and the effect of mobile phase conditions on HPLC separation of gonyautoxins （GTXs） were discussed. Fluorescent intensity of GTXs had different sensitivity to reaction system pH, temperature, formamide concentration and ammonium formate concentration. Therefore, the optimum post-column derivatization conditions were determined to be derivatization with pH 7.3-7.5, 70 mmol/L periodic acid/20% formamide solution containing 0.12 mol/L potassium hydrate and 0.75 mol/L ammonium formate with a flow rate of 0.8 mL/min at 50 ℃. Methanol concentration, sodium heptanesulfonate concentration, pH and phosphate concentration bad significant impacts on retention time and separation of each tested GTX and optimized to be 1%, 1.5 mmol/L, 7.3 and 10 mmol/L, respectively. The sensitivity of detection for GTX1, GTX3 and GTX4 by the HPLC method was 4.7-, 3,4- and 3.8-fold increased as compared to the Oshima method, whereas no obvious difference in the sensitivity of detection for GTX2 was observed.

关 键 词： 麻痹性贝毒 膝沟藻毒素 柱后衍生 高效液相色

领　　域： [生物学]