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首页> 外文期刊>Toxins >Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method Coupled with Dispersive Solid-Phase Extraction for Simultaneous Quantification of Eight Paralytic Shellfish Poisoning Toxins in Shellfish
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Development and Validation of a Liquid Chromatography-Tandem Mass Spectrometry Method Coupled with Dispersive Solid-Phase Extraction for Simultaneous Quantification of Eight Paralytic Shellfish Poisoning Toxins in Shellfish

机译：液相色谱-串联质谱联用分散固相萃取同时定量检测贝类中八种麻痹性贝类毒素的方法的建立和验证

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In this study, a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for simultaneous determination of eight paralytic shellfish poisoning (PSP) toxins, including saxitoxin (STX), neosaxitoxin (NEO), gonyautoxins (GTX1–4) and the N -sulfo carbamoyl toxins C1 and C2, in sea shellfish. The samples were extracted by acetonitrile/water (80:20, v / v ) with 0.1% formic and purified by dispersive solid-phase extraction (dSPE) with C18 silica and acidic alumina. Qualitative and quantitative detection for the target toxins were conducted under the multiple reaction monitoring (MRM) mode by using the positive electrospray ionization (ESI) mode after chromatographic separation on a TSK-gel Amide-80 HILIC column with water and acetonitrile. Matrix-matched calibration was used to compensate for matrix effects. The established method was further validated by determining the linearity ( R 2 ≥ 0.9900), average recovery (81.52–116.50%), sensitivity (limits of detection (LODs): 0.33–5.52 μg·kg ?1 ; limits of quantitation (LOQs): 1.32–11.29 μg·kg ?1 ) and precision (relative standard deviation (RSD) ≤ 19.10%). The application of this proposed approach to thirty shellfish samples proved its desirable performance and sufficient capability for simultaneous determination of multiclass PSP toxins in sea foods.
机译：在这项研究中，开发了一种高效液相色谱-串联质谱（HPLC-MS / MS）方法，用于同时测定八种麻痹性贝类中毒（PSP）毒素，包括毒毒素（STX），新毒素（NEO）和淋病毒素（ GTX1-4）和N-磺基氨基甲酰基毒素C1和C2，在海洋贝类中。样品用含0.1％甲酸的乙腈/水（80:20，v / v）萃取，并用C18二氧化硅和酸性氧化铝通过分散固相萃取（dSPE）纯化。在TSK-gel Amide-80 HILIC色谱柱上用水和乙腈进行色谱分离后，通过使用正电喷雾电离（ESI）模式在多反应监测（MRM）模式下进行目标毒素的定性和定量检测。基质匹配的校准用于补偿基质效应。确定线性（R 2≥0.9900），平均回收率（81.52–116.50％），灵敏度（检测限（LOD）：0.33–5.52μg·kg？1;定量限（LOQ））进一步验证了所建立的方法：1.32–11.29μg·kg？1）和精度（相对标准偏差（RSD）≤19.10％）。该建议方法在三十个贝类样品中的应用证明了其理想的性能和足够的能力同时测定海鲜中的多类PSP毒素。

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