摘要
建立了能同时测定碘克沙醇关键中间体5-乙酰氨基-N,N-双(2,3-二羟丙基)-2,4,6-三碘-1,3-苯二甲酰胺及其5种有关物质的HPLC法。采用柱长150mm内径4.6mm和粒径3.5μm的色谱柱(柱温30℃),以0.05%磷酸水和乙腈作为流动相,流速1.0mL·min^(-1),在240nm波长处检测。6种物质分离度均大于1.5,相关系数r均大于等于0.9986,检出限浓度为0.008~0.019μg·mL^(-1),定量限浓度为0.026~0.063μg mL^(-1);加标平均回收率在90.0%~96.5%,RSD(n=9)均≤5.9%,人员比对的重复实验数据表明方法重复性好、中间精密度高,微调色谱条件后的进样数据证明方法耐用性良好。在3批1中间体样品的测定中,3均未检出,2、45.6含量均小于0.07%,最大未知单杂含量均小于0.09%,总杂含量均小于0.44%。因此,建立的方法简便、可靠,能同时对1及2~6进行准确测定。
A HPLC method was established for the simultaneous determination of the key intermediate 5-Acetamino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triodo-1,3-phthalamide and its five related substances in Iodixanol.A chromatographic column with a column length of 150 mm,inner diameter of 4.6 mm,and particle size of 3.5μm was used(column temperature of 30℃),with 0.05%phosphoric acid water and acetonitrile as mobile phases at a flow rate of 1.0 mL·min^(-1),and detected at a wavelength of 240 nm.The separation degree of all six substances was greater than 1.5,the correlation coefficient r was greater than or equal to 0.9986,and the detection limit concentration was 0.008~0.019μg·mL^(-1),with a quantification limit concentration of 0.026~0.063μg mL^(-1);The average recovery rate of spiked samples ranged from 90.0%to 96.5%,with RSD(n=9)≤5.9%.The repeated experimental data compared by personnel showed that the method had good repeatability and high intermediate precision.The injection data after fine-tuning the chromatographic conditions proved that the method had good durability.In the determination of 3 batches of intermediate samples,3 were not detected,and the contents of 2,4,5,and 6 were all less than 0.07%.The maximum un-known impurity content was less than 0.09%,and the total impurity content was less than 0.44%.Therefore,the established method is simple and reliable,and can accurately determine 1 and 2~6 simultaneously.
作者
王茴茴
王瑞华
郭宇彤
徐东强
吝红娟
程青芳
WANG Hui-hui;WANG Rui-hua;GUO Yu-tong;XU Dong-qiang;LIN Hong-juan;CHENG Qing-fang(School of Pharmacy,Jiangsu Ocean University,Lianyungang 222005,China;Jiangsu Yutian Pharmaceutical Co.,Ltd.,Lianyungang 222000,China)
出处
《化学研究与应用》
CAS
北大核心
2024年第5期1178-1184,共7页
Chemical Research and Application
基金
连云港市科技成果转化"揭榜挂帅"专项资金项目(CA202101)资助
研究生科研与实践创新计划项目(KYCX2023-53)资助。
关键词
碘克沙醇
中间体
杂质
含量测定
iodixanol
intermediate
impurity
content determination
