Lawrence J F, Wong B
Food Research Division, Bureau of Chemical Safety, Ottawa, Ont., Canada.
J Chromatogr A. 1996 Dec 6;755(2):227-33. doi: 10.1016/s0021-9673(96)00598-5.
Using manganese dioxide as a solid-phase oxidant, a post-column HPLC reactor for paralytic shellfish poison toxins was constructed and evaluated. Operating parameters such as reaction temperature and pH, flow-rate, reactor column size, and MnO2 particle size were studied. Based on a 3:1 signal-to-noise ratio the limits of detection for the non-hydroxylated toxins were in the sub-nanogram range, while the hydroxylated toxins were ten times less detectable. The limit of detection for saxitoxin was about 0.1 ng per injection. The repeatability of replicate injections was < or = 10% (relative standard deviation). The system was used to analyze extracts of shellfish and plankton yielding results that were in agreement with those obtained by established analytical methods. Extracts of shellfish contaminated at the regulatory limit of 0.8 microgram/g were successfully analyzed.
以二氧化锰作为固相氧化剂，构建并评估了一种用于麻痹性贝类毒素的柱后高效液相色谱反应器。研究了诸如反应温度和pH值、流速、反应器柱尺寸以及二氧化锰颗粒尺寸等操作参数。基于3:1的信噪比，非羟基化毒素的检测限在亚纳克范围内，而羟基化毒素的可检测性则低十倍。石房蛤毒素的检测限约为每次进样0.1纳克。重复进样的重复性小于或等于10%（相对标准偏差）。该系统用于分析贝类和浮游生物提取物，所得结果与通过既定分析方法获得的结果一致。成功分析了受0.8微克/克监管限量污染的贝类提取物。
