Lawrence J F, Ménard C, Cleroux C
Health Protection Branch, Food Research Division, Ottawa, ON, Canada.
J AOAC Int. 1995 Mar-Apr;78(2):514-20.
A liquid chromatographic (LC) method employing prechromatographic oxidation for the determination of paralytic shellfish poison (PSP) toxins was evaluated. A number of changes to an earlier method resulted in improved separation and quantitation of most PSP analogues. Modification of the periodate oxidation reaction for the N-hydroxy-containing toxins led to improved sensitivity and stability of the products, enabling automated overnight analyses. These changes also enabled quantitation of gonyautoxins 1 and 4 (together) in the presence of gonyautoxins 2 and 3. Decarbamoylsaxitoxin can be identified and quantitated after peroxide oxidation. A cleanup step using a strong-anion-exchange column removed the C toxins and B-2 from the extracts and enabled a more accurate quantitation of gonyautoxins 1 and 4 and neosaxitoxin. Chiral chromatography, employing a reversed-phase column and chiral mobile-phase additives (copper-proline complex), was briefly evaluated for the separation of the oxidation products of the isomer pairs, gonyautoxins 1 and 4 and gonyautoxins 2 and 3. A comparison of the method with the mouse bioassay for the determination of PSP in lobster hepatopancreas (58 samples) showed a reasonable correlation (0.90) over a concentration range of 40-500 micrograms/100 g (saxitoxin equivalents), although the LC results were consistently higher than the mouse bioassay values by about 40%.
对一种采用色谱前氧化法测定麻痹性贝类毒素（PSP）的液相色谱（LC）方法进行了评估。对早期方法进行的一些改进使得大多数PSP类似物的分离和定量得到了改善。对含N-羟基毒素的高碘酸盐氧化反应进行改进后，产物的灵敏度和稳定性得到提高，从而能够进行自动化的过夜分析。这些改进还使得在存在膝沟藻毒素2和3的情况下能够对膝沟藻毒素1和4（一起）进行定量。过氧化后可鉴定并定量脱氨甲酰基石房蛤毒素。使用强阴离子交换柱的净化步骤可从提取物中去除C毒素和B-2，并能更准确地定量膝沟藻毒素1和4以及新石房蛤毒素。简要评估了采用反相柱和手性流动相添加剂（铜-脯氨酸络合物）的手性色谱法对异构体对膝沟藻毒素1和4以及膝沟藻毒素2和3的氧化产物的分离效果。将该方法与用于测定龙虾肝胰腺中PSP的小鼠生物测定法（58个样品）进行比较，结果表明，在40 - 500微克/100克（石房蛤毒素当量）的浓度范围内，两者具有合理的相关性（0.90），尽管LC结果始终比小鼠生物测定值高约40%。
