Turner Andrew D, Lewis Adam M, Rourke Wade A, Higman Wendy A
J AOAC Int. 2014 Mar-Apr;97(2):380-90. doi: 10.5740/jaoacint.sgeturner.
An interlaboratory ring trial was designed and conducted by the Centre for Environment, Fisheries, and Aquaculture Science to investigate a range of issues affecting the analysis of a candidate Pacific oyster paralytic shellfish toxin reference material. A total of 21 laboratories participated in the study and supplied results using one or more of three instrumental methods, specifically precolumn oxidation (Pre-COX) LC with fluorescence detection (FLD; AOAC Official Method 2005.06), postcolumn oxidation (PCOX) LC-FLD (AOAC Official Method 2011.02), and hydrophilic interaction LC/MS/MS. Each participant analyzed nine replicate samples of the oyster tissue in three separate batches of three samples over a period of time longer than 1 week. Results were reported in a standardized format, reporting both individual toxin concentrations and total sample toxicity. Data were assessed to determine the equivalency of the two AOAC LC methods and the LC/MS/MS method as well as an assessment of intrabatch and interbatch repeatability and interlaboratory reproducibility of each method. Differences among the results reported using the three methods were shown to be statistically significant, although visual comparisons showed an overlap between results generated by the majority of tests, the exception being the Pre-COX quantitation of N-hydroxylated toxins in post ion-exchange fractions. Intralaboratory repeatability and interlaboratory reproducibility were acceptable for most of the results, with the exception of results generated from fractions. The results provided good evidence for the acceptable performance of the PCOX method for the quantitation of C toxins. Overall the study showed the usefulness of interlaboratory analysis for the characterization of paralytic shellfish poisoning matrix reference materials, highlighting some issues that may need to be addressed with further method assessment at individual participant laboratories.
环境、渔业和水产养殖科学中心设计并开展了一项实验室间循环试验，以调查一系列影响太平洋牡蛎麻痹性贝类毒素候选参考物质分析的问题。共有21个实验室参与了该研究，并使用三种仪器方法中的一种或多种提供了结果，具体为带有荧光检测的柱前氧化（Pre-COX）液相色谱法（FLD；AOAC官方方法2005.06）、柱后氧化（PCOX）液相色谱 - 荧光检测法（AOAC官方方法2011.02）和亲水相互作用液相色谱/质谱/质谱法。每位参与者在超过1周的时间内，分三批、每批三个样品对牡蛎组织的九个重复样品进行了分析。结果以标准化格式报告，同时报告了单个毒素浓度和样品总毒性。对数据进行了评估，以确定两种AOAC液相色谱法和液相色谱/质谱/质谱法的等效性，以及对每种方法的批内和批间重复性及实验室间再现性的评估。尽管视觉比较显示大多数测试结果之间存在重叠，但使用这三种方法报告的结果之间的差异在统计学上具有显著性，唯一的例外是离子交换后馏分中N-羟基化毒素的Pre-COX定量。除馏分产生的结果外，大多数结果的实验室内重复性和实验室间再现性是可接受的。这些结果为PCOX法对C毒素定量的可接受性能提供了有力证据。总体而言，该研究表明实验室间分析对于麻痹性贝类中毒基质参考物质表征的有用性，突出了一些可能需要在各参与实验室通过进一步方法评估来解决的问题。
