Harju Kirsi, Rapinoja Marja-Leena, Avondet Marc-André, Arnold Werner, Schär Martin, Burrell Stephen, Luginbühl Werner, Vanninen Paula
VERIFIN (Finnish Institute for Verification of the Chemical Weapons Convention), Department of Chemistry, University of Helsinki, P.O. Box 55, A. I. Virtasen aukio 1 FI-00014, Finland.
Federal Department of Defence, Civil Protection and Sport, SPIEZ LABORATORY, Austrasse 1, Spiez CH-3700, Switzerland.
Toxins (Basel). 2015 Nov 25;7(12):4868-80. doi: 10.3390/toxins7124853.
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).
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）及一些选定的麻痹性贝类毒素（PSP）类似物进行了鉴定和定量。针对LC-MS/MS分析，对贻贝样品的提取和净化方法进行了优化。所开发的方法应用于EQuATox项目（建立潜在生物恐怖主义风险生物毒素检测质量保证体系）能力验证（PT）中均质贻贝样品的分析。来自八个国家的十个实验室参与了STX PT。通过将产物离子谱和保留时间与参考标准品进行比较，对天然污染贻贝样品中的PSP毒素进行鉴定。通过向有毒贻贝提取物中加入参考标准品，利用LC-MS/MS获得定量结果。与官方AOAC（美国官方分析化学家协会）2005.06方法（柱前氧化高效液相色谱-荧光检测法，HPLC-FLD）测定结果相比，结果在±1的z分数范围内。
