Background: An ultrahigh-performance LC (UHPLC)–tandem MS (MS/MS) method for determination of paralytic shellfish poisoning toxins and tetrodotoxin (TTX) in bivalve molluscs was developed. To be used for regulatory testing, it needed to be validated through collaborative study. Objective: The aim was to conduct a collaborative study with 21 laboratories, using results to assess method performance. Methods: Study materials incorporated shellfish species mussels, oysters, cockles, scallops, and clams and were assessed to demonstrate stability and homogeneity. Mean concentrations determined by participants for blind duplicate samples were used to assess reproducibility, repeatability, and trueness. Results: Method performance characteristics were excellent following statistical assessment of participant data, with method trueness showing excellent method accuracy against expected values. No significant difference was found in the trueness results determined by different chromatographic column types. Acceptability of the between-laboratory reproducibility for individual analytes was evidenced by >99% of valid Horwitz ratio values being less than the 2.0 limit of acceptability. With excellent linearity and sensitivity fit-for-purpose over a range of mass spectrometer instruments, the UHPLC-MS/MS method compared well against other detection methods. It includes additional paralytic shellfish toxin (PST) analogues as well as TTX, which, to date, have not been incorporated into any other hydrophilic marine toxin official method of analysis. Conclusions: The results from this study demonstrate that the method is suitable for the analysis of PST analogues and TTX in shellfish tissues and is recommended as an official alternative method of analysis for regulatory control. Highlights: A new mass spectrometric method for PST and TTX has been validated successfully through collaborative study.

中文翻译：

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超高效液相色谱-串联质谱法测定贻贝，牡蛎，蛤，蛤和扇贝中的麻痹性贝类毒素和河豚毒素：合作研究。

背景：建立了一种用于测定双壳贝类软体动物中麻痹性贝类毒素和河豚毒素（TTX）的超高效液相色谱（UHPLC）-串联质谱（MS / MS）方法。要用于法规测试，需要通过合作研究进行验证。目的：目的是与21个实验室进行合作研究，使用结果评估方法的性能。方法：研究材料结合了贝类物种的贻贝，牡蛎，蛤，扇贝和蛤，并进行了评估，以证明其稳定性和同质性。由参与者确定的盲样品的平均浓度用于评估可重复性，可重复性和真实性。结果：在对参与者数据进行统计评估之后，方法性能特征非常出色，方法真实性显示了相对于预期值的出色方法准确性。在不同色谱柱类型确定的真实性结果中未发现显着差异。大于99％的有效Horwitz比值小于2.0的可接受限度，证明了各个分析物的实验室间重现性的可接受性。UHPLC-MS / MS方法在一系列质谱仪仪器上具有出色的线性度和适合特定用途的灵敏度，因此与其他检测方法相比非常出色。它包括其他麻痹性贝类毒素（PST）类似物以及TTX，迄今为止，它们尚未被纳入任何其他亲水性海洋毒素官方分析方法中。结论：这项研究的结果表明该方法适用于贝类组织中PST类似物和TTX的分析，并被推荐作为监管控制的官方替代分析方法。要点：通过合作研究，已成功验证了用于PST和TTX的新质谱方法。