高效液相色谱法同时测定盐酸乐卡地平中的10种有关物质  

Simultaneous determination of ten related substances in lercanidipine hydrochloride by high performance liquid chromatography

作　　者：杨毅[1,2] 黄锦钿 刘婷婷 赵春杰 YANG Yi;HUANG Jintian;LIU Tingting;ZHAO Chunjie(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;Shenzhen Salubris Pharmaceuticals Co.,Ltd.,Shenzhen 518102,China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]深圳信立泰药业股份有限公司,广东深圳518102

出　　处：《沈阳药科大学学报》2021年第3期264-271,283,共9页Journal of Shenyang Pharmaceutical University

摘　　要：目的采用高效液相色谱法,建立一种盐酸乐卡地平原料药有关物质的检查方法,可同时测定原料药中的10种有关物质。方法以十八烷基硅烷键合硅胶为色谱填充剂(GL Inertsil ODS-3V,250 mm×4.6 mm,5μm),流动相A:0.15 mol·L^(-1)高氯酸钠溶液-乙腈(体积比61∶39)、流动相B:乙腈,进行梯度洗脱;检测波长240 nm;柱温35℃;流速1.3 mL·min^(-1);进样量15μL;运行时间45 min。结果杂质A、B、C、D、E、F、G、H、I和J的检测限分别为4.58、8.25、11.0、14.9、2.80、10.4、8.73、4.07、4.06和11.3μg·L^(-1),定量限分别为13.9、25.0、33.4、45.1、8.47、31.6、26.5、12.3、12.3和34.3μg·L^(-1),线性范围分别为0.0139~1.73、0.0250~1.72、0.0334~1.65、0.0451~1.71、0.00847~1.76、0.0316~1.66、0.0265~1.68、0.0123~1.73、0.0123~1.74和0.0343~1.70 mg·L^(-1),杂质A、B、C、D、E、F、G、H、I和J的回收率范围分别为102.6%~105.7%、96.8%~102.0%、95.9%~100.9%、95.1%~103.7%、95.7%~101.4%、96.9%~99.9%、97.3%~100.6%、99.1%~102.1%、98.6%~101.4%和99.4%~110.6%,专属性、重复性、中间精密度、耐用性良好,符合验证要求。结论本方法灵敏度好,操作简单,可准确、快速地检测盐酸乐卡地平中的有关物质。Objective To establish a method for the determination of the related substances in lercanidipine hydrochloride by HPLC.Method The method was performed on GL Inertsil ODS-3 V column(250 mm×4.6 mm,5μm)with the mobile phase A of sodium perchlorate solution(0.15 mol·L^(-1))-acetonitrile(V∶V=61∶39)and the mobile phase B of acetonitrile,gradient elution.The wavelength was 240 nm,flow rate was 1.3 mL·min^(-1),column temperature was 35℃,injection volume was 15μL,operation time was 45 min.Results The detection limits of impurities A,B,C,D,E,F,G,H,I and J were 4.58,8.25,11.0,14.9,2.80,10.4,8.73,4.07,4.06 and 11.3μg·L^(-1),respectively.The quantitative limits of impurities A,B,C,D,E,F,G,H,I and J were 13.9,25.0,33.4,45.1,8.47,31.6,26.5,12.3,12.3 and 34.3μg·L^(-1),respectively.The linear ranges of impurities A,B,C,D,E,F,G,H,I and J were 0.0139-1.73,0.0250-1.72,0.0334-1.65,0.0451-1.71,0.00847-1.76,0.0316-1.66,0.0265-1.68,0.0123-1.73,0.0123-1.74 and 0.0343-1.70 mg·L^(-1),respectively.The recoveries of impurities A,B,C,D,E,F,G,H,I and J were 102.6%-105.7%,96.8%-102.0%,95.9%-100.9%,95.1%-103.7%,95.7%-101.4%,96.9%-99.9%,97.3%-100.6%,99.1%-102.1%,98.6%-101.4%and 99.4%-110.6%,respectively.The specificity,repeatability,accuracy of intermediates and durability were good,which conform to the requirement.Conclusion This method can accurately detect the impurities in the lercanidipine hydrochloride,which has the advantages of simple operation,high sensitivity,good accuracy and feasibility.

关 键 词：盐酸乐卡地平 有关物质 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]