摘要
采用质谱、核磁、红外及紫外对河豚毒素样品进行结构确证,采用柱后衍生高效液相荧光法对该纯度标准样品进行定值并进行了均匀性、稳定性检验。标准样品经国内6个具有分析资质的实验室进行协同定值,定值结果为99.45%,其扩展不确定度(95%置信区间)为0.51%。该标准样品达到国家标准样品的技术要求,可用于有关河豚毒素的方法校正和质量控制。
The structure of tetrodotoxin certified reference material was comfirmed by mass spectrometry, ^1H NMR, ^13C NMR, infrared spectroscopy and ultraviolet spectroscopy. The checking of homegeneity, stability test and value certification were systematically studied by post column derivation HPLC - FLD. A cooperative certification was conducted with 6 qualified laboratories. The results showed that the certified value of the reference material of tetrodotoxin purity was 99.45% with the expanded uncertainty of 0.51% and confidence coefficient of 95%. The reference material can conform to the technical requirement of the certified reference material. The materials were intended for use in the method validation and quality control regarding tetrodotoxin.
出处
《化学分析计量》
CAS
2010年第2期7-11,共5页
Chemical Analysis And Meterage
基金
厦门市海洋渔业局资助专项项目(厦海渔合[2009]10号)
