Kelly S S, Bishop A G, Carmody E P, James K J
Chemistry Department, Cork RTC, Bishopstown, Ireland.
J Chromatogr A. 1996 Oct 18;749(1-2):33-40. doi: 10.1016/0021-9673(96)00448-7.
The rare diarrhetic shellfish toxin, dinophysistoxin-2 (DTX-2), was isolated from the digestive glands of mussels (Mytilus edulis). This was achieved by chromatography on silica and Sephadex LH-20 followed by reversed-phase solid phase extraction and semi-preparative high-performance liquid chromatography (HPLC) with an Ultremex C18 column. Using 1-bromoacetylpyrene (BAP), as a precolumn derivatisation reagent, the diarrhetic shellfish toxins, okadaic acid (OA), dinophysistoxin-1 (DTX-1) and DTX-2, were determined by HPLC with fluorimetric detection. Derivatisation using BAP was compared with 9-anthryldiazomethane (ADAM) and, although the latter exhibited a four-fold better sensitivity, the BAP method gave fewer artefact peaks from reagent decomposition. The limits of detection of OA and DTX-2 were 0.4 ng on-column using BAP, which permits this method to be used for the regulatory control of these toxins in shellfish.
从贻贝（紫贻贝）的消化腺中分离出了罕见的腹泻性贝类毒素——鳍藻毒素-2（DTX-2）。这是通过硅胶柱色谱和葡聚糖凝胶LH-20柱色谱，随后进行反相固相萃取以及使用Ultremex C18柱的半制备高效液相色谱（HPLC）实现的。使用1-溴乙酰芘（BAP）作为柱前衍生试剂，通过带有荧光检测的HPLC测定腹泻性贝类毒素——冈田酸（OA）、鳍藻毒素-1（DTX-1）和DTX-2。将使用BAP的衍生化方法与9-蒽重氮甲烷（ADAM）进行了比较，尽管后者的灵敏度高四倍，但BAP方法产生的试剂分解伪峰较少。使用BAP时，OA和DTX-2的柱上检测限为0.4 ng，这使得该方法可用于贝类中这些毒素的监管控制。
