CAJ | 학술논문

通过半制备高效液相色谱法制备了双烯雌酚纯度标准物质，采用液相色谱-质谱联用技术、核磁共振氢谱、碳谱和红外光谱对制得的原料化合物进行定性分析；然后采用HPLC多家实验室联合定值法对双烯雌酚纯度标准物质中的有机主成分含量进行测定，对双烯雌酚纯度标准物质的均匀性、稳定性进行检验，并对水分、灰分、挥发性物质、无机金属元素含量进行分析；最后对双烯雌酚纯度标准物质的不确定度进行评定。结果表明：该标准物质均匀性良好，稳定期不少于12个月；标准物质中水分、灰分、挥发性物质、无机金属元素的含量均小于0．1％；标准物质的定值结果为99．4％，扩展不确定度为0.6％（k＝2）。
통과반제비고효액상색보법제비료쌍희자분순도표준물질，채용액상색보-질보련용기술、핵자공진경보、탄보화홍외광보대제득적원료화합물진행정성분석；연후채용HPLC다가실험실연합정치법대쌍희자분순도표준물질중적유궤주성분함량진행측정，대쌍희자분순도표준물질적균균성、은정성진행검험，병대수분、회분、휘발성물질、무궤금속원소함량진행분석；최후대쌍희자분순도표준물질적불학정도진행평정。결과표명：해표준물질균균성량호，은정기불소우12개월；표준물질중수분、회분、휘발성물질、무궤금속원소적함량균소우0．1％；표준물질적정치결과위99．4％，확전불학정도위0.6％（k＝2）。
In this paper,first,certified reference material (CRM)for the purity determination of dienestrol was prepared by means of semi-preparative high-performance liquid chromatography.Next,a qualitative analysis of the raw materials was performed by using liquid chromatography-mass spectrometry,1H NMR,13C NMR and infrared spectroscopy.Then,the content of organic main ingredients in the prepared CRM was determined via the multi-lab certification with HPLC,and the homogeneity and stability of the CRM were measured.Moreover,the contents of water,ash,volatile materials and inorganic elements were analyzed,with an uncertainty evaluation of the CRMbe-ing finally carried out.The results indicate that (1 )the prepared CRM possesses good homogeneity and is of a sta-ble storage period of 12 months;(2)the contents of water,ash,volatile materials and inorganic elements in the prepared CRM of dienestrol are all less than 0.1%;and (3)the prepared CRM is of a certified purity of 99.4%and a relative expanded uncertainty of 0.6% (k=2).