Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry.
Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry.
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DOI：
10.3390/toxins7124853
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发表时间：
2015-11-25
期刊：
影响因子：
4.2
通讯作者：
Vanninen P
中科院分区：
文献类型：
--
作者：
Harju K;Rapinoja ML;Avondet MA;Arnold W;Schär M;Burrell S;Luginbühl W;Vanninen P
采用液相色谱-串联质谱法（LC-MS/MS）对贻贝样品中的石房蛤毒素（STX）和麻痹性贝毒（PSP）类似物进行了定性和定量分析。对贻贝样品的提取和纯化方法进行了优化，并用于LC-MS/MS分析。所开发的方法被应用于分析的均质化贻贝样品的能力测试（PT）内的EQuATox项目（建立质量保证检测潜在的生物恐怖主义风险的生物毒素）。来自8个国家的10个实验室参加了STX PT。通过与参比标准品的产物离子谱和保留时间的比较，鉴定了自然污染的贻贝样品中的PSP毒素。通过在有毒贻贝提取物中加入参比标准品，采用LC-MS/MS获得定量结果。当与使用官方AOAC（官方分析化学家协会）方法2005.06，柱前氧化高效液相色谱-荧光检测（HPLC-FLD）测量的结果相比时，结果在±1的z评分范围内。
Saxitoxin (STX) and some selected paralytic shellfish poisoning (PSP) analogues in mussel samples were identified and quantified with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Sample extraction and purification methods of mussel sample were optimized for LC-MS/MS analysis. The developed method was applied to the analysis of the homogenized mussel samples in the proficiency test (PT) within the EQuATox project (Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk). Ten laboratories from eight countries participated in the STX PT. Identification of PSP toxins in naturally contaminated mussel samples was performed by comparison of product ion spectra and retention times with those of reference standards. The quantitative results were obtained with LC-MS/MS by spiking reference standards in toxic mussel extracts. The results were within the z-score of ±1 when compared to the results measured with the official AOAC (Association of Official Analytical Chemists) method 2005.06, pre-column oxidation high-performance liquid chromatography with fluorescence detection (HPLC-FLD).