一种检测麻痹性贝毒的高效液相色谱法
麻痹性贝毒,,高效液相色谱，柱后衍生，麻痹性贝毒,摘要,关键词,1引言,2材料与方法,3结果和讨论,References
摘 要提出了一种利用高效液相色谱法同时分析麻痹性贝毒GTX组分和NEO/dcSTX/ STX组分的方法。本法仅使用了一种缓冲溶液作为流动相，在Inertsil C83色谱柱(250 mm×4.6 mm, 5 μm)上，采用梯度改变乙腈在流动相中的比例和流速，一次进样可同时定性及定量待测试样中的上述全部毒素组分。该缓冲溶液为9.0 mmol/L磷酸铵缓冲溶液(pH=7.2)，含有2.8 mmol/L的庚烷磺酸钠。色谱分离过程首先以纯水相缓冲溶液进行等度洗脱，在16.5~19 min向流动相中梯度加入1.5%的乙腈，加速GTX3和GCX2的洗脱，以避免GTX2的色谱峰与乙腈的溶剂峰重叠，随后从19 min开始加大流动相中乙腈的比例为8.5%，以缩短边缘组分的保留时间。荧光检测器的激发波长和发射波长分别设为330 nm和390 nm。用本方法分析染毒的华贵栉孔扇贝和近江牡蛎，证实了本方法对PSP毒素具有良好的分析测定效果。
关键词 高效液相色谱，柱后衍生，麻痹性贝毒
Method to Determine Paralytic Shellfish Poisoning by High Performance Liquid Chromatography
Jiang Tianjiu 1,4, Jiang Tao 2, Xie Liqi 3 ,Ouyang Shan3, Zhou Yamin3
(Ji′nan University, Department of Environmental Engineering1,College of Life Science and Technology2, Guangzhou 510631)
(Inspect Center of Import and Export Food, Shenzhen EntryExit Inspect and Quarantine Bureau, Shenzhen 518067)
(College of Life Science and Technology, South China Normal University, Guangzhou 510632)
Abstract A method in which only one buffer is used as mobile phase , was proposed to determine all gonyautoxin (GTXs) and NEO/decarbamoyl soxitoxin (dcSTX)/STX. The buffer contains 2.8 mmol/L sodium heptanesulfonate in 9 mmol/L ammonium phosphate buffer ( pH 7.2) and an Inertsil C83 column (250 mm×4.6 mm, 5 μm) was used. There were two gradient elutions in a chromatographic run. The first from 100% buffer to 98.5% buffer and 1.5% acetoitrile at 16.5 min decreases the retention times of GTX3 and GTX2 and also avoids the merge of the peaks of GTX2 and the solvent peak. The second with 8.5% acetonitrile from 19 to 45 min allows a rapid elution of the latest compouds. The spectrofluorometric detector is set at λex=330 nm and λem=390 nm. The method has been applied to the analysis of samples contaminated with PSP toxins with satisfactory result. The regression equation, the linear range and the detection limit are given. ......
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