4,9-脱水河豚毒素国家标准样品的研制

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。

Development of Anhydrotetrodotoxin Certiifed Reference Material

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.