Janecek M, Quilliam M A, Lawrence J F
Institute for Marine Biosciences, National Research Council of Canada, Halifax, Nova Scotia.
J Chromatogr. 1993 Aug 6;644(2):321-31. doi: 10.1016/0021-9673(93)80715-k.
Periodate oxidation of the toxins responsible for paralytic shellfish poisoning (PSP) yields fluorescent purines suitable for trace analysis by reversed-phase LC. Mobile phases containing perfluorinated acids, such as heptafluorobutyric acid, as ion-pair agents were found to provide high capacity factors for the oxidized products. Gradient elution on a microbore column with large volume injections and fluorescence detection permitted the detection of femtomole quantities of PSP toxins. A fully automated pre-column oxidation procedure was developed for an LC autosampler system in order to improve precision and allow unattended analyses. The complete method was applied successfully to various samples, including shellfish and toxic phytoplankton.
对导致麻痹性贝类中毒（PSP）的毒素进行高碘酸盐氧化，可产生适用于反相液相色谱痕量分析的荧光嘌呤。发现含有全氟代酸（如七氟丁酸）作为离子对试剂的流动相能为氧化产物提供高容量因子。在微径柱上进行梯度洗脱，采用大体积进样和荧光检测，可检测到飞摩尔量的PSP毒素。为液相色谱自动进样器系统开发了一种全自动柱前氧化程序，以提高精密度并实现无人值守分析。该完整方法已成功应用于各种样品，包括贝类和有毒浮游植物。
