液相色谱_荧光检测_麻痹性贝毒_质谱_

过氧化氢柱前荧光衍生化液相色谱法测定麻痹性贝毒的研究

http://www.100md.com 《分析化学》 2006年第7期

液相色谱,荧光检测,麻痹性贝毒,质谱,,液相色谱，荧光检测，麻痹性贝毒，质谱,摘要,关键词,1引言,2实验部分,3结果与讨论,Referen

     摘要 液相色谱荧光检测法(LCFLD)测定贝类样品中石房蛤毒素(STX)和decarbamoylsaxitoxin(dcSTX)。样品经30 mmol/L HAc超声提取，C18固相萃取柱净化，2%碱性H2O2荧光衍生，C18色谱柱(4.6 mm×250 mm， 5 μm)分离，以乙腈0.1 mol/L甲酸铵溶液(5∶95，V/V)作流动相，流速1.0 mL/min。结果表明，STX和dcSTX衍生物在7min内获得完全分离。在空白样品中添加标准品使浓度0.01～2.0 μg/g，得到峰面积与浓度呈良好线性，线性相关系数>0.998。添加浓度在0.1、0.8和1.6 μg/g的回收率为87%～97%(n=8)；相对标准偏差为8%～13%。方法检出限(S/N=3)分别为STX 1.0 ng/g和dcSTX 0.3 ng/g。另外，采用四极杆飞行时间质谱(QTOFMS)对STX和dcSTX衍生物进行了结构解析。

     关键词 液相色谱，荧光检测，麻痹性贝毒，质谱

    Determination of Paralytic Shellfish Poisoning Toxins by Liquid Chromatography with Fluorescence Detection Using Precolumn Derivatization with Hydrogen Peroxide Oxidation

    Chen Di, Fang Xiaoming， Fan Xiang, Tang Yifeng, Yong Kelan

    (School of Life Science, Shanghai University, Shanghai 200436)

    (Shanghai ExitEntry Inspection and Quarantine Bureau, Shanghai 200135)

    Abstract Saxitoxin (STX) and decarbamoylsaxitoxin (dcSTX) were determined by liquid chromatography with fluorescence detection. A shellfish tissue was extracted with 30 mmol/L HAc under ultrasonication, and cleanup of extract was accomplished by solidphase extraction with a C18 cartridge. Fluorescence derivatization of STX and dcSTX was used with 2% alkaline H2O2 solution. Chromatographic separation was carried out on a C18 column(4.6 mm×250 mm ......

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