关键词: 双烯雌酚, 标准物质, 高效液相色谱法, 定值, 不确定度

Abstract:

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).

Key words: dienestrol, certified reference material, high- performance liquid chromatography, certification, uncer-tainty