碘佛醇主成分异构体及其有关物质同时分离检测和结构确证  

Simultaneous Separation and Detection of Principal Component Isomers and Related Substances in Ioversol Bulk Drug

作　　者：李婕[1] 王英 黄海伟[1] 刘毅[1] 何兰[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]秦皇岛市食品药品检验中心,河北秦皇岛066300

出　　处：《中国药学杂志》2016年第17期1488-1492,共5页Chinese Pharmaceutical Journal

基　　金：国家"重大新药创制"科技重大专项资金资助项目(2011ZX09303-001)

摘　　要：目的建立超高效液相色谱=质谱联用法（UPLC—MS）对碘佛醇主成分异构体及有关物质同时进行分离检测和结构鉴定。方法采用Watefs ACQUITY UPLC^TM BEH C8（2．1mm×100mm，1．7μm）色谱柱，流动相为乙腈-0．1％甲酸溶液（3：97），检测波长为254nm；电喷雾离子源，检测模式为正离子，锥孔电压为80V。结果碘佛醇4个光学异构体及有关物质分离良好，并且通过了质谱、紫外光谱和液相色谱的确证。碘佛醇、杂质Ⅰ和杂质Ⅱ分别在0．5～52．8、0．2～9．3、0．5～28-4μg·mL^-1内呈良好的线性关系（r=0．9999）；检出限分别为0．2、0．08、0．2μg·mL^-1。结论该方法简便、灵敏、准确，可用于碘佛醇主成分异构体及有关物质的同时分离检测。OBJECTIVE To establish a UPLC-MS method for the separation and detection of principal component isomers and related substances in ioversol bulk drug. METHODS The separation was ped＇ormed on a Waters ACQUITY UPLCTM BEH Cs column （2.1mm×100mm,1.7μm）, the mobile phase consisted of acetonitrile-0. 1% formic acid in water （3： 97） ,and the detection wavelength was set at 254 nm. The identification of isomers and impurities in ioversol bulk drug was performed with a triple-quadrupole mass spectrometer, with an electrospray ionization （ESI） source in the positive ion mode, and the cone voltage was set at 80 V. RESULTS The four optical isomers and related substances were seperated well, and their structures were confirmed by MS,UV, and RP-UP- LC. The linear ranges of ioversol, impurity Ⅰ , and impurity Ⅱ were 0. 5 - 52.8, 0. 2 - 9. 3, and 0. 5 - 28.4 μg·mL^-1, respectively （r = 0. 999 9 ） ; the detection limits of ioversol, impurity Ⅰ , and impurity Ⅱ were 0. 2, 0. 08, and 0. 2μg·mL^-1 , respectively. CONCLUSION The method is simple, sensitive, and accurate, can be used to separate and determine the principal component isomers and related substances in ioversol bulk drug.

关 键 词：碘佛醇 光学异构体 有关物质 超高效液相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]