【摘要】 目的建立聚山梨酯80的8类化学组分的对照品的制备方法,对获得的对照品进行纯度测定。方法分别合成聚氧乙烯山梨醇酐油酸酯和聚氧乙烯异山梨醇油酸酯,结合中低压制备色谱和Flash柱进行分离纯化,利用核磁共振谱、红外、拉曼、质谱等技术鉴定结构,用高效液相色谱技术测定聚山梨酯80单一化学组分对照品的纯度。结果分离鉴定了聚山梨酯80的8类化学组分,纯度均大于99.5%,满足作为对照品的要求。结论首次建立以定向合成并结合中低压色谱技术,快速、准确制备聚山梨酯80化学组分对照品的方法,并且首次公布了这8类化学组分的波谱数据。更多还原

【Abstract】 OBJECTIVE To establish a new method for the preparation and purity determination of the reference standards for eight types of chemical compositions in polysorbate 80.METHODS Polyoxyethylene 24 sorbitan oleate and polyoxyethylene 12 isosorbide oleate were synthesized respectively.Medium and low pressure preparative chromatography and flash column were used to separate and purify the constituents,and their structures were elucidated by IR,Raman,MS,1H-NMR and 13C-NMR.RESULTS Eight single chemical compositions of polysorbate 80 were obtained,the purities of which were greater than 99.5% tested by HPLC,meeting the requirement as a reference standard.CONCLUSION A directed synthesis together with a medium and low pressure preparative chromatography method is established for the first time which can accurately and rapidly prepare the reference standards for eight chemical compositions of polysorbate 80.And for the first time the spectral data of the eight chemical components were reported.更多还原