Mass spectrometric methods for the quantitative and qualitative analyses of algal biotoxins are often complicated by co-eluting compounds that present analytically as interferences. This issue is particularly critical for organic polyamines, where co-eluting materials can suppress the formation of cations during electrospray ionization. Here we present an extraction procedure designed specifically to overcome matrix-derived ion suppression of algal toxins in samples of Lyngbya wollei, a filamentous benthic algae known to produce several saxitoxin analogues. Lyngbya wollei samples were collected from a large, persistent harmful algal bloom in Lake Wateree, SC. Six known Lyngbya wollei-specific toxins (LWT1–6) were successfully resolved and quantified against saxitoxin using hydrophilic interaction liquid chromatography coupled with triple quadrupole and quadrupole time-of-flight mass spectrometry. The parent ions [M²⁺ – H⁺]⁺ were observed for LWTs 1–6 and the [M]²⁺ ion was observed for LWT5. High resolution mass spectra and unique fragmentation ions were obtained for LWTs 1–6. A dilution factor of 50 resulted in a linear calibration of saxitoxin in the algae matrix. Ion suppression was resolved by sample dilution, which led to linear, positive correlations between peak area and mass of the extracted sample (R² > 0.96). Optimized sample extraction method and instrument parameters are presented.

用于藻类生物毒素定量和定性分析的质谱方法通常由于共洗脱化合物而变得复杂，这些化合物在分析中表现为干扰。对于有机多胺而言，此问题尤为关键，在有机多胺中，共洗脱材料可以抑制电喷雾电离过程中阳离子的形成。在这里，我们介绍了一种提取程序，该提取程序专门设计用于克服Lyngbya wollei（一种已知可产生数种毒素毒素类似物的丝状底栖藻类）样品中藻类毒素的基质衍生离子抑制。Lyngbya wollei样品是从南卡罗来纳州Wateree的大型持续性有害藻华中采集的。六种已知的Lyngbya wollei亲水相互作用液相色谱结合三重四极杆和四极杆飞行时间质谱法成功地分离和定量了针对毒素的特异毒素（LWT1-6）。LWT 1–6观察到母离子[M ²⁺ – H ⁺ ] ⁺，LWT5观察到[M] ²⁺离子。LWT 1–6获得了高分辨率质谱和独特的碎片离子。稀释系数为50导致藻类基质中的沙毒素的线性校准。通过样品稀释解决了离子抑制问题，这导致了峰面积与提取样品质量之间的线性正相关（R ²> 0.96）。提出了优化的样品提取方法和仪器参数。