2023·12本刊特稿1ModernChemicalResearch当代化工研究高效液相色谱法测定碘海醇原料药中的杂质含量＊熊先水1,2江丹丹1邢乐2廖蓉蓉2肖晶晶2刘昆明1*（1.江西理工大学材料冶金化学学部江西3410002.江西兄弟医药有限公司江西332700）摘要：建立了碘海醇API中杂质G和杂质S（同分异构体杂质）的HPLC分析方法。方法：色谱柱为AgilentZORBAXSB-Aq型C18柱（4.6×250mm，5μm），流动相为乙腈-0.1%磷酸溶液（4:96），柱温为25℃，检测波长为254nm，流速为1.0mL/min，进样量为10μL，进样时间为60min。结果：碘海醇杂质G在0.0692～2.799μg/mL的范围内呈线性，碘海醇杂质S在0.0188～3.852μg/mL的范围内呈线性，线性相关系数均大于0.995，检测下限均不高于0.05μg/mL。准确度实验表明，两种杂质的平均回收率分别为98.4%和116.4%。供试品溶液在室温放置49h内，两种杂质均十分稳定。不同柱温、流动相、流速及色谱柱条件下，测定结果未见明显差异。结论：本文所建立的高效液相色谱测试方法简单准确、重复性好、灵敏度高，可用于碘海醇原料药中的杂质G和异构体杂质S含量测定。关键词：碘海醇；高效液相色谱；杂质；含量测定中图分类号：R917文献标识码：ADOI：10.20087/j.cnki.1672-8114.2023.12.001DeterminationofImpuritiesinIohexolAPIbyHighPerformanceLiquidChromatographyXiongXianshui1,2,JiangDandan1,XingLe2,LiaoRongrong2,XiaoJingjing2,LiuKunming1*(1.FacultyofMaterialsMetallurgyandChemistry,JiangxiUniversityofScienceandTechnology,Jiangxi,3410002.JiangxiBrothersPharmaceuticalCo.,Ltd.,Jiangxi,332700)Abstract：ToestablishedaHPLCprotocolforthedeterminationofimpuritiesGandSiniohexol.Method:AgilentZORBAXSB-AqC18column(4.6×250mm,5μm)wasadopted,withthemobilephasecomposedofacetonitrile-0.1%phosphoricacid(4:96),andthecolumntemperaturewas25℃.Thedetectionwavelengthwas254nm,andtheflowratewas1.0mL/min,settingtheinjectionvolumeas10μLandtheinjectiontimeas60min.Results:theiohexolimpurityGwaslinearintherangeof0.0692μg/mLto2.799μg/mL,andtheiohexolimpuritySwaslinearintherangeof0.0188μg/mLto3.852μg/mL,withthelinearcorrelationcoefficientswerebothlargerthan0.995,andthelimitofdetectionwereallbelow0.05μg/mL.Theaccuracytestshowedthattheaveragerecoveriesofthetwoimpuritiesare98.4%and116...
