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) 。

In this paper,first,certified reference material (CRM) for the purity determination of dienestrol wasprepared by means of semi- preparative high- performance liquid chromatography. Next,a qualitative analysis of theraw materials was performed by using liquid chromatography- mass spectrometry,1H NMR,13C NMR and infraredspectroscopy.Then,the content of organic main ingredients in the prepared CRM was determined via the multi- labcertification with HPLC,and the homogeneity and stability of the CRM were measured. Moreover, the contents ofwater,ash,volatile materials and inorganic elements were analyzed,with an uncertainty evaluation of the CRM be-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 theprepared 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).