4,9-脱水河豚毒素国家标准样品的研制 |
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引用本文: | 陈伟珠,;谢全灵,;张怡评,;洪专,;方华,;洪碧红,;易瑞灶. 4,9-脱水河豚毒素国家标准样品的研制[J]. 化学分析计量, 2014, 0(3): 1-4 |
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作者姓名: | 陈伟珠, 谢全灵, 张怡评, 洪专, 方华, 洪碧红, 易瑞灶 |
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作者单位: | [1]国家海洋局第三海洋研究所,福建厦门 361005; [2]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,福建厦门 361005 |
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基金项目: | 广东海洋经济发展区域示范项目(GD2012-D01-001);海洋生物产业化中试技术研发公共服务平台(12PZP001SF10);厦门市重大科技创新平台项目(3502220111001);国家科技支撑计划(NO.2011BAK04809) |
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摘 要: | 研制4,9-脱水河豚毒素国家标准样品。以河豚鱼卵巢为原料,提取制备4,9-脱水河豚毒素,采用红外光谱(IR)、高分辨质谱和核磁共振谱(NMR)进行结构确证。样品分装成140瓶后,采用柱后衍生–高效液相荧光法进行均匀性、稳定性检验和定值分析。从样品中随机抽取15瓶进行均匀性检验,经F检验表明在95%的置信区间范围内样品均匀性良好;稳定性考察按照40℃加速试验稳定性(6个月)进行,结果表明在考察期间内样品稳定性良好;标准样品经国内8家具有分析资质的实验室进行协同定值,并评定了定值结果的不确定度,4,9-脱水河豚毒素标准样品定值结果为97.77%,相对扩展不确定度为0.4%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关脱水河豚毒素的方法校正和质量控制。
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关 键 词: | -脱水河豚毒素 标准样品 柱后衍生–高效液相荧光色谱法 定值 不确定度 |
Development of Anhydrotetrodotoxin Certiifed Reference Material |
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Affiliation: | Chen Weizhu, Xie Quanling, Zhang Yiping, Hong Zhuan, Fang Hua, Hong Bihong, Yi Ruizao (1. The Third Institute of Oceanography of the State Oceanic Administration, Xiamen 361005, China ; 2. Department of Chemistry and Key Laboratory Chemical Biology of Fujian Province, Xiamen University, Xiamen 361005, China) |
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Abstract: | 4,9-anhydrotetrodotoxin certified reference material was developed. 4,9-anhydrotetrodotoxin was made from the ovarium of pufferfish. The structure of anhydrotetrodotoxin certified reference material was comfirmed by mass spectrometry and NRM,infrared spectroscopy (IR). 4,9-anhydrotetrodotoxin was divided into 140 bottles. The homogeneity and stability testing and quantitative analysis were evaluated by post column derivation high performance liquid chromatography-fluorescent detection (HPLC-FLD) method. According to analysis procedure of homogeneity,15 bottles of sample were randomly taken from 140 bottles,and the results were validated by F-test statistical method. The stability inspection was carried on the short-term(6 months),and the results indicated that the period for anhydrotetrodotoxin of storage was 6 months at 40℃. A cooperative certification was conducted with 8 qualified laboratories. The certified purity value of the reference material of 4,9-anhydrotetrodotoxin was 97.77%with relative expaned uncertainty of 0.40%(k=1.96). The reference material can conform to the technical requirement of the certified reference material. The material was intended for use in the method validation and quality control regarding anhydrontetrodotoxin. |
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Keywords: | 4,9-anhydrotetrodotoxin certified reference material post column derivation-HPLC-FLD certification uncertainty |
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