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Agilent ZORBAX SB-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。
To established a HPLC protocol for the determination of impurities G and S in iohexol.Method:Agilent ZORBAX SB-Aq C18 column(4.6×250 mm,5μm)was adopted,with the mobile phase composed of acetonitrile-0.1%phosphoric acid(4:96),and the column temperature was 25℃.The detection wavelength was 254 nm,and the flow rate was 1.0 mL/min,setting the injection volume as 10μL and the injection time as 60 min.Results:the iohexol impurity G was linear in the range of 0.0692μg/mL to 2.799μg/mL,and the iohexol impurity S was linear in the range of 0.0188μg/mL to 3.852μg/mL,with the linear correlation coefficients were both larger than 0.995,and the limit of detection were all below 0.05μg/mL.The accuracy test showed that the average recoveries of the two impurities are 98.4%and 116.4%,respectively.The two impurities were stable when the test solution was placed at room temperature for 49 h.Changing the column temperature,mobile phase,flow rate,and replacing the chromatographic column exhibited no effect on the detection results of related impurities.Conclusion:The established HPLC method possesses simplicity,accuracy,reproducibility and sensitivity,is suitable for the content detection of impurities G and S in iohexol API.
作者
熊先水
江丹丹
邢乐
廖蓉蓉
肖晶晶
刘昆明
Xiong Xianshui;Jiang Dandan;Xing Le;Liao Rongrong;Xiao Jingjing;Liu Kunming(Faculty of Materials Metallurgy and Chemistry,Jiangxi University of Science and Technology,Jiangxi,341000;Jiangxi Brothers Pharmaceutical Co.,Ltd.,Jiangxi,332700)
出处
《当代化工研究》
CAS
2023年第12期1-4,共4页
Modern Chemical Research
基金
江西省自然科学面上基金“基于动态络合平衡的新型ate-络合物参与的铁催化偶联反应研究”(项目编号:20212BAB203013)
江西省自然科学基金青年项目“五(六)元环醚的多组分开环及串联反应研究”(项目编号:20202BABL213007)
大学生创新创业训练计划项目“基于新型荧光探针对富硒土壤-农作物系统中有机硒迁移规律的研究”(项目编号:202110407006)。
