CAJ | 학술논문

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。
연제4，9-탈수하돈독소국가표준양품。이하돈어란소위원료，제취제비4，9-탈수하돈독소，채용홍외광보（IR）、고분변질보화핵자공진보（NMR）진행결구학증。양품분장성140병후，채용주후연생-고효액상형광법진행균균성、은정성검험화정치분석。종양품중수궤추취15병진행균균성검험，경F검험표명재95%적치신구간범위내양품균균성량호；은정성고찰안조40℃가속시험은정성（6개월）진행，결과표명재고찰기간내양품은정성량호；표준양품경국내8가구유분석자질적실험실진행협동정치，병평정료정치결과적불학정도，4，9-탈수하돈독소표준양품정치결과위97.77%，상대확전불학정도위0.4%(k=1.96)。해표준양품체도국가표준양품적기술요구，가용우유관탈수하돈독소적방법교정화질량공제。
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.