摘要
目的 建立一种超高效液相色谱(UPLC)法测定创新药LW33中有关物质,并与其高效液相色谱法(HPLC)进行对比研究。方法 UPLC法采用Waters Acquity UPLC BEH C18(2.1 mm×100 mm,1.7 μm)色谱柱,流速0.21 mL·min^(-1);HPLC法采用SHISEIDO CAPCELL PAK C18(4.6 mm×250 mm,5 μm)色谱柱,流速1.0 mL·min^(-1);两种方法均以水溶液(用冰醋酸调pH值至3.0)(A)-甲醇(B)为流动相进行梯度洗脱,检测波长257 nm,柱温25℃。结果 UPLC法和HPLC法测定的有关物质在一定范围内均呈现良好线性,准确度、精密度和样品测定结果基本无差异;UPLC法运行时间为16 min,HPLC法运行时间为40 min,UPLC法溶剂使用量为HPLC法的1/10。结论 UPLC和HPLC 两种方法的准确度、精密度、线性等验证结果以及样品测定结果基本一致,UPLC法与HPLC法相比,分析快速,节省溶剂,适用于快速检测LW33中的有关物质,提高研发的效率。
Objective To develop and validate a stable UPLC method for the determination of related substances in LW33,and to compare the results with those by HPLC method.Methods A gradient UPLC system was used in the quantitative analysis of related substances on Waters Acquity UPLC BEH C18 column (2.1 mm×100 mm,1.7 μm).Mobile phase A consisted of aqueous solution (adjusting pH to 3.0 with glacial acetic acid),and mobile phase B consisted of methanol,under a flow rate of 0.21 mL·min^(-1).An HPLC method was conducted on SHISEIDO CAPCELL PAK C18 column (4.6 mm×250 mm,5 μm),based on the same mobile phases as the UPLC method,with a flow rate of 1.0 mL·min^(-1).The wavelength and column temperature were set at 257 nm and 25℃,respectively for both methods.Results The linear relationship between the concentration and peak areas of the compounds was all satisfactory.The analytical validation (accuracy and repeatability) and detection results for impurities showed no significant difference in both methods.UPLC method showed shorter analysis time (2/5 of HPLC method),and less solvent used (1/10 that of HPLC method).Conclusion Both methods showed similar results.The UPLC method is more time saving,and solvent saving,which is suitable for rapid detection of related substances in LW33,with better efficiency.
作者
张容华
杨放
郑艾妮
鲍颖霞
赖烨才
余华
陈绮玲
王健松
ZHANG Rong-hua;YANG Fang;ZHENG Ai-ni;BAO Ying-xia;LAI Ye-cai;YU Hua;CHEN Qi-ling;WANG Jian-song(Baiyunshan Pharmaceutical General Factory,Guangzhou Baiyunshan Pharmaceutical Group Co.,Ltd.,Guangzhou 510515;Key Laboratory of Key Technology Research on Chemical Raw Materials and Preparations of Guangdong,Guangzhou 510515;State Key Laboratory of Quality Research in Chinese Medicine,Institute of Chinese Medical Sciences,University of Macao,Macao 999078)
出处
《中南药学》
CAS
2022年第10期2379-2384,共6页
Central South Pharmacy
基金
科技部重大新药创制专项(No.2019ZX09301-104)
广东省科技厅粤澳科技创新联合资助项目(No.2021A0505080010)
澳门科学技术发展基金(No.FDCT 0058/2020/AGJ)。
