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作 者:王霄旸[1,2] 张可煜[2] 张丽芳[2] 费陈忠[2] 王米[2] 薛飞群[2] 杭太俊[1]
机构地区:[1]中国药科大学药物分析教研室,江苏南京210009 [2]中国农业科学院上海兽医研究所中国农业科学院兽药安全评价与兽药残留研究重点开放实验室农业部动物寄生虫病学重点开放实验室,上海200241
出 处:《中国兽医科学》2016年第5期623-629,共7页Chinese Veterinary Science
基 金:公益性行业(农业)科研专项经费项目(201303038)
摘 要:建立了分离鉴定头孢喹肟中同分异构体杂质的UPLC与TOF及MS/MS联用方法。以乙腈-1m L/L甲酸水为流动相进行梯度洗脱,经RP18色谱柱分离,通过电喷雾串联质谱正离子模式在线检测,使得头孢喹肟及其同分异构体杂质获得有效分离,主成分和其同分异构体杂质的保留时间分别为4.9 min和4.5 min,同时它们的二级质谱产物离子信息及其裂解方式呈现明显的差异。本试验初步建立了分离及鉴定头孢喹肟同分异构体杂质的色谱质谱检测方法,为硫酸头孢喹肟原料药和制剂的有关物质研究及检测奠定了基础。Sensitive and specific methods for the determination of isomeric impurity of cefquinome were established with UPLC-TOF and UPLC-MS/MS. UPLC separation experiments were performed on a RP18 column with acetonrtrile-0.1% formic acid water solution as mobile phase by gradient e]ution. The ana- lytes were determined by electrospray ionization tandem mass spectrometry in a position mode. The chromatogram and mass spectra of cefquinome and its isomeric impurity were obtained by UPLC-MS/MS, of which the retention times were 4.90 min and 4.50 min, respectively. The ion information of MS/MS of the products and their cleavage patterns showed obvious differences. In this paper the method was estab- lished to separate and identify the isomer and impurities of raw material and the preparation of the raw materials and the preparation of Cefquinome.
关 键 词:硫酸头孢喹肟 同分异构体 超高效液相 飞行时间质谱 电喷雾质谱
分 类 号:S859.796[农业科学—临床兽医学]
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