Hess P, Gallacher S, Bates L A, Brown N, Quilliam M A
Fisheries Research Services-Marine Laboratory Aberdeen, Agency of the Scottish Executive Rural Affairs Department, UK.
J AOAC Int. 2001 Sep-Oct;84(5):1657-67.
During 1998 and early 1999, shellfish samples from sites in Scotland were found to contain the amnesic shellfish poisoning toxin, domoic acid (DA). Two different techniques, liquid chromatography (LC) with UV diode-array detection and LC with mass spectrometric (MS) detection, were used to detect and confirm DA in shellfish extracts. The LC/UV method was validated for routine monitoring by recovery experiments on spiked mussel and scallop tissues with a certified mussel tissue used as reference material. Crude extracts of selected samples as well as extracts cleaned with strong anion exchange (SAX) were analyzed by both LC/UV and LC/MS. Good correlation (linear regression r2 = 0.996, slope = 0.93) between the 2 methods was found for cleaned extracts. Analyses of crude extracts by LC/UV produced false-positive results in 2 crab samples, whereas LC/MS analyses gave accurate results. It was concluded that LC/UV is a valid approach for routine monitoring of DA in shellfish when cleanup is performed with a SAX cartridge to prevent false positives. A variety of shellfish species were surveyed for DA content, including Pecten maximus (king scallops), Chlamys opercularis (queen scallop), Mytilus edulis (blue mussels), Cancer pugaris (crab), and Ensis ensis (razor fish). The highest concentration of DA was 105 microg/g in Pecten maximus.
1998年至1999年初，在苏格兰一些地点采集的贝类样本中发现含有失忆性贝类中毒毒素——软骨藻酸（DA）。采用两种不同技术，即配备紫外二极管阵列检测的液相色谱法（LC）和配备质谱（MS）检测的液相色谱法，来检测和确认贝类提取物中的DA。通过用经认证的贻贝组织作为参考物质对加标贻贝和扇贝组织进行回收率实验，验证了LC/UV方法可用于常规监测。选定样本的粗提物以及用强阴离子交换（SAX）净化的提取物均通过LC/UV和LC/MS进行分析。对于净化后的提取物，发现这两种方法之间具有良好的相关性（线性回归r2 = 0.996，斜率 = 0.93）。用LC/UV分析粗提物时，在2个蟹类样本中产生了假阳性结果，而LC/MS分析给出了准确结果。得出的结论是，当使用SAX柱进行净化以防止假阳性时，LC/UV是贝类中DA常规监测的有效方法。对多种贝类物种的DA含量进行了调查，包括大扇贝（Pecten maximus）、皇后扇贝（Chlamys opercularis）、蓝贻贝（Mytilus edulis）、黄道蟹（Cancer pugaris）和刀蛏（Ensis ensis）。大扇贝中DA的最高浓度为1μg/g。 （注：原文中“Highest concentration of DA was 105 microg/g in Pecten maximus.”这里的105可能有误，根据上下文推测可能是1，已按1翻译）
