HPLC法测定N-叔丁氧羰基-5,7-二氯-1,2,3,4-四氢异喹啉-6-羧酸中的有关物质  

Determination of Related Substances in N-tert-Butoxycarbonyl-5,7-dichloro-1,2,3,4-tetrahydroisoquinoline-6-carboxylic Acid by HPLC

作　　者：李亚苹 刘絮 林丽娅 张福利[2] 何永富 LI Yaping;LIU Xu;LIN Liya;ZHANG Fuli;HE Yongfu(School of Chemistry and Chemical Engineering,Shanghai University of Engineering and Science,Shanghai 201620;Shanghai Institute of Pharmaceutical Industry Co.,Ltd.,Shanghai 201203;Zhejiang Boxiao Biopharmaceutical Co.,Ltd.,Hangzhou 310014)

机构地区：[1]上海工程技术大学化学化工学院,上海201620 [2]上海医药工业研究院有限公司,上海201203 [3]浙江博崤生物制药有限公司,浙江杭州310014

出　　处：《中国医药工业杂志》2024年第1期107-112,共6页Chinese Journal of Pharmaceuticals

摘　　要：建立了HPLC法测定立他司特的关键起始物料N-叔丁氧羰基-5,7-二氯-1,2,3,4-四氢异喹啉-6-羧酸(1)中的有关物质。采用Thermo Acclaim~(TM) Mixed-Mode WAX-1柱(4.6 mm×250 mm,5μm),以30 mmol/L磷酸二氢钾溶液和乙腈(体积比95∶5)为流动相A,以乙腈和四氢呋喃(体积比80∶20)为流动相B,梯度洗脱。流速为0.9 mL/min,柱温为30℃,检测波长为205 nm,进样量为50μL。结果显示,主成分与各杂质间分离度良好,且在相应浓度范围内线性关系良好。平均回收率(n=9)为96.4%~105.6%,RSD均≤5.1%。该方法操作简单、准确、可靠,适用于1中有关物质的测定。An HPLC method was established to determine the related substances in N-tert-butoxycarbonyl-5,7-dichloro-1,2,3,4-tetrahydroisoquinoline-6-carboxylic acid(1),a key starting material for liftegrast.A Thermo Acclaim^(TM) Mixed-Mode WAX-1 column(4.6 mm×250 mm,5μm)was used,and the analysis was carried out in the gradient elution mode with 30 mmol/L potassium dihydrogen phosphate solution-acetonitrile(95:5)as mobile phase A,and acetonitrile-tetrahydrofuran(80:20)as mobile phase B.The flow rate was 0.9 mL/min,the column temperature was 30℃,the detection wavelength was 205 nm,and the injection amount was 50μL.The results showed that the separation between the main component and various impurities was good,and it was linear for the main component and various impurities in the corresponding concentration ranges.The average recoveries(n=9)were 96.4%-105.6%,with the RSDs less than 5.1%.This method is easy to operate,accurate,and reliable,which is suitable for the determination of related substances in1.

关 键 词：N-叔丁氧羰基-5 7-二氯-1 2 3 4-四氢异喹啉-6-羧酸 立他司特 高效液相色谱 有关物质 

分 类 号：R917[医药卫生—药物分析学]