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河豚毒素标准样品的研制
引用本文:陈伟珠,易瑞灶,谢全灵,张怡评,洪专,洪碧红.河豚毒素标准样品的研制[J].化学分析计量,2010,19(2):7-11.
作者姓名:陈伟珠  易瑞灶  谢全灵  张怡评  洪专  洪碧红
作者单位:1. 国家海洋局第三海洋研究所海洋生物资源化学与化工中心,厦门,361005;厦门大学化学化工学院化学系,化学生物学福建省重点实验室,厦门,361005
2. 国家海洋局第三海洋研究所海洋生物资源化学与化工中心,厦门,361005
基金项目:厦门市海洋渔业局资助专项项目 
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。

关 键 词:河豚毒素  标准物质  柱后衍生高效液相荧光法  均匀性  稳定性  定值  不确定度

DEVELOPMENT OF TETRODOTOXIN CERTIFIED REFERENCE MATERIAL
Chen Weizhu,Yi Ruizao,Xie Quanling,Zhang Yiping,Hong Zhuan,Hong Bihong.DEVELOPMENT OF TETRODOTOXIN CERTIFIED REFERENCE MATERIAL[J].Chemical Analysis And Meterage,2010,19(2):7-11.
Authors:Chen Weizhu  Yi Ruizao  Xie Quanling  Zhang Yiping  Hong Zhuan  Hong Bihong
Institution:1. The Third Institute of Oceanography of The State Oceanic Administration, Xiamen 361005, China; 2. Department of Chemistry and Key Laboratory for Chemical Biology of Fujian Province, Xiamen University, Xiamen 361005, China)
Abstract: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.
Keywords:tetrodotoxin  certified reference material  HPLC - FLD  homegeneity  stability  certification  uncertainty
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