van Egmond H P, Mouriño A, Burdaspal P A, Boenke A
National Institute of Public Health and the Environment, Laboratory for Residue Analysis, Bilthoven, The Netherlands.
J AOAC Int. 2001 Sep-Oct;84(5):1668-76.
A project was undertaken to develop mussel reference materials that were certified for their mass fractions of saxitoxin and decarbamoyl-saxitoxin. Fifteen laboratories from various European countries participated. Three of these had major responsibility for substantial parts of the work and overall coordination of the project. The project involved 4 main activities: (1) procurement and characterization of calibrants; (2) improvement of analytical methodology; (3) preparation of reference materials, including homogeneity and stability studies; (4) 2 interlaboratory studies and a certification exercise. The joint activities resulted in 3 homogeneous and stable reference materials: 2 lyophilized mussel materials with and without naturally incurred paralytic shellfish poisoning (PSP) toxins, and a saxitoxin enrichment solution. The reference materials were certified with respect to their saxitoxin and decarbamoyl-saxitoxin content. The lyophilized mussel material with PSP toxins (CRM 542) contained <0.07 mg saxitoxin x 2HCl/kg and 1.59 +/- 0.20 mg decarbamoyl-saxitoxin x 2HCl/kg. The lyophilized mussel material without PSP toxins (CRM 543) contained <0.07 mg saxitoxin x 2HCl/kg and <0.04 mg decarbamoyl-saxitoxin x 2HCl/kg. The certified value of the saxitoxin mass fraction in the saxitoxin enrichment solution (CRM 663) was 9.8 +/- 1.2 microg/g.
开展了一个项目，旨在开发贻贝参考物质，这些物质的石房蛤毒素和脱氨甲酰基石房蛤毒素质量分数经过认证。来自欧洲各国的15个实验室参与其中。其中三个实验室主要负责该项目大部分工作及整体协调。该项目涉及4项主要活动：（1）校准物的采购与特性鉴定；（2）分析方法的改进；（3）参考物质的制备，包括均匀性和稳定性研究；（4）两项实验室间研究及一次认证活动。这些联合活动产生了3种均匀且稳定的参考物质：2种冻干贻贝物质，一种含有天然产生的麻痹性贝类毒素（PSP），另一种不含，以及一种石房蛤毒素富集溶液。这些参考物质的石房蛤毒素和脱氨甲酰基石房蛤毒素含量经过了认证。含有PSP毒素的冻干贻贝物质（CRM 542）每千克含石房蛤毒素x2HCl<0.07毫克及脱氨甲酰基石房蛤毒素x2HCl 1.59±0.20毫克。不含PSP毒素的冻干贻贝物质（CRM 543）每千克含石房蛤毒素x2HCl<0.07毫克及脱氨甲酰基石房蛤毒素x2HCl<0.04毫克。石房蛤毒素富集溶液（CRM 663）中石房蛤毒素质量分数的认证值为9.8±1.2微克/克。
