摘要
建立了HPLC-CAD法测定舒更葡糖钠(1)原料药中的7种有关物质(2~8)。色谱柱采用Poroshell 120 SB-C8柱(4.6 mm×150 mm,2.7μm),流动相A为0.5%甲酸溶液,B为甲醇,线性梯度洗脱,流速为0.5 mL/min,柱温为35℃。电雾式检测器(CAD)雾化器温度为35℃,过滤常数为3.6 s,数据采集速率为5 Hz。结果表明,3在5~300 μg/mL内线性关系良好,1及其他有关物质均在2~40 μg/mL内线性关系良好。1原料药及各杂质(2~8)的定量限为0.985~1.145 μg/mL,检测限为0.493~0.573 μg/mL;2~8的平均回收率(n=9)为95.6%~99.4%,RSD为1.21%~3.32%。该方法准确、重现性好、精密度高,可检测1原料药中的有关物质,为1的质量控制提供了可靠的检测方法。
An HPLC-CAD method was established for the determination of seven related substances(2-8)in sugammadex sodium(1)bulk drug.The Poroshell 120 SB-C_8 column(4.6 mm×150 mm,2.7μm)was used,and the analysis was carried out in the linear gradient elution mode with 0.5%formic acid solution as mobile phase A,and methanol as mobile phase B.The flow rate was 0.5 mL/min and the column temperature was 35℃.The temperature of the atomizer of the charged aerosol detector(CAD)was 35℃,the filtration constant was 3.6 s,and the data acquisition rate was 5 Hz.The results showed that it was linear for 3 in the range of 5-300μg/mL,and it was linear for 1 bulk drug and other related substances in the range of 2-40μg/mL.The LOQs and LODs of 1-8 were 0.985-1.145μg/mL and 0.493-0.573μg/mL,respectively.The average recoveries(n=9)of 2-8 were 95.6%-99.4%,with the RSDs of 1.21%-3.32%.This method is accurate,reproducible,and highly precise,which can be used to detect the related substances in 1bulk drug,and also provides a reliable detection method for the quality control of 1.
作者
冯中
朱冬青
庞余江
朱志祥
宋玉鹏
张贵民
FENG Zhong;ZHU Dongqing;PANG Yujiang;ZHU Zhixiang;SONG Yupeng;ZHANG Guimin(International Pharmaceutical Engineering Lab.in Shandong Province,Shandong New Time Pharmaceutical Co.,Ltd.,Linyi 273400;School of Medicine and Pharmacy,Ocean University of China,Qingdao 266003)
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2023年第5期785-790,共6页
Chinese Journal of Pharmaceuticals
基金
国家手性制药工程技术研究中心(2016GGH4528)给予资助。
