A simple, rapid UHPLC-MS/MS method has been developed and optimised for the quantitation of microcystins and nodularin in wide variety of sample matrices. Microcystin analogues targeted were MC-LR, MC-RR, MC-LA, MC-LY, MC-LF, LC-LW, MC-YR, MC-WR, [Asp3] MC-LR, [Dha7] MC-LR, MC-HilR and MC-HtyR. Optimisation studies were conducted to develop a simple, quick and efficient extraction protocol without the need for complex pre-analysis concentration procedures, together with a rapid sub 5 min chromatographic separation of toxins in shellfish and algal supplement tablet powders, as well as water and cyanobacterial bloom samples. Validation studies were undertaken on each matrix-analyte combination to the full method performance characteristics following international guidelines. The method was found to be specific and linear over the full calibration range. Method sensitivity in terms of limits of detection, quantitation and reporting were found to be significantly improved in comparison to LC-UV methods and applicable to the analysis of each of the four matrices. Overall, acceptable recoveries were determined for each of the matrices studied, with associated precision and within-laboratory reproducibility well within expected guidance limits. Results from the formalised ruggedness analysis of all available cyanotoxins, showed that the method was robust for all parameters investigated. The results presented here show that the optimised LC-MS/MS method for cyanotoxins is fit for the purpose of detection and quantitation of a range of microcystins and nodularin in shellfish, algal supplement tablet powder, water and cyanobacteria. The method provides a valuable early warning tool for the rapid, routine extraction and analysis of natural waters, cyanobacterial blooms, algal powders, food supplements and shellfish tissues, enabling monitoring labs to supplement traditional microscopy techniques and report toxicity results within a short timeframe of sample receipt. The new method, now accredited to ISO17025 standard, is simple, quick, applicable to multiple matrices and is highly suitable for use as a routine, high-throughout, fast turnaround regulatory monitoring tool.

已经开发了一种简单，快速的UHPLC-MS / MS方法，并已优化了该方法，用于定量各种样品基质中的微囊藻毒素和结核菌素。靶向的微囊藻毒素类似物是MC-LR，MC-RR，MC-LA，MC-LY，MC-LF，LC-LW，MC-YR，MC-WR，[Asp3] MC-LR，[Dha7] MC-LR， MC-HilR和MC-HtyR。进行了优化研究，以开发简单，快速，高效的提取方案，而无需进行复杂的预分析浓缩程序，并且快速进行了不到5分钟的色谱分离，分离了贝类和藻类补充剂片剂，水和蓝细菌中的毒素绽放样品。按照国际准则，对每种基质-分析物组合进行了充分的方法性能特征验证研究。发现该方法是特定的，并且在整个校准范围内都是线性的。发现与LC-UV方法相比，在检测，定量和报告范围方面的方法灵敏度得到了显着提高，并且适用于四种基质中的每一种的分析。总体而言，确定了每种所研究基质的可接受的回收率，相关的精密度和实验室内的重现性均在预期的指导范围内。对所有可用氰毒素的形式耐用性分析的正规化结果表明，该方法对所研究的所有参数均具有鲁棒性。此处显示的结果表明，针对毒素的优化LC-MS / MS方法适用于检测和定量贝类，藻类补充剂片剂，水和蓝细菌。该方法为快速，常规地提取和分析天然水，蓝藻水华，藻粉，食品补充剂和贝类组织提供了宝贵的预警工具，使监测实验室可以补充传统的显微镜技术并在短时间内采集样品的毒性结果收据。现在已通过ISO17025标准认证的新方法简单，快速，适用于多种基质，非常适合用作常规，高通量，快速周转法规监控工具。使监测实验室可以补充传统的显微镜技术，并在短时间内收到样品后报告毒性结果。现在已通过ISO17025标准认证的新方法简单，快速，适用于多种基质，非常适合用作常规，高通量，快速周转法规监控工具。使监测实验室可以补充传统的显微镜技术，并在短时间内收到样品后报告毒性结果。现在已通过ISO17025标准认证的新方法简单，快速，适用于多种基质，非常适合用作常规，高通量，快速周转法规监控工具。