自制异噁草酮标准物质纯度、均匀性及稳定性测定

Determinations of purity,uniformity and stability for self-prepared working standard of clomazone

通过有机合成制得异草酮原药 ,采用柱层析分离技术 ,以硅胶为填料 ,V乙酸乙酯∶V石油醚 (沸点 3 0～ 60℃ ) =1∶4为展开剂(Rf=0 5 )作进一步纯化、分离。优选了实验条件 ,应用高效液相色谱法及气相色谱法对所制备的标准物质进行纯度测定 (>99% ) ,测定结果具有一致性。以高效液相色谱法进行均匀性及稳定性考察 。

Clomazone reference material was prepared and purified by column chromatography with silica gel as stationary phase and ethyl acetate/petroleum ether(boiling point 30～60℃) at a ratio of one to four as mobile phase( R f=0.5).The test conditions were optimized,and the purities were determined by both HPLC and GC with a good consistency of values exceeding 99%.The homogeneity and stability were examined by HPLC,and the results were satisfactory.