258.4RP-HPLC法测定拉米夫定的含量及有关物质
作 者:李萌 刘有平 鲁静 邸欣
LI Meng, LIU You - ping, LU Jing, DI Xin ( School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China )
机构地区:沈阳药科大学药学院,沈阳110016
出 处:《药物分析杂志》 CAS CSCD 2009年第7期 1216-1219页,共4页
Chinese Journal of Pharmaceutical Analysis
摘 要:目的:建立测定拉米夫定含量及有关物质的RP-HPLC方法。方法:进行拉米夫定含量测定及有关物质检查时,采用Diamonsil C18柱(200mm×4.6mm,5μm),流动相为0.025mol·L^-1醋酸铵溶液(pH3.9±0.1)-甲醇(90∶10),流速为1.0mL·min^-1,检测波长为277nm;进行拉米夫定对映体纯度检查时,采用CYCLOBOND I2000RSP柱(250mm×4.6mm,5μm),流动相为0.05mol·L^-1醋酸铵溶液(pH3.9±0.1)-甲醇(95∶5),流速为0.8mL·min^-1,检测波长为270nm。结果:拉米夫定与其他杂质能较好分离,拉米夫定浓度在5.0~50.0μg·mL^-1范围内线性关系良好(r=0.9997),平均回收率为100.1%(RSD=0.69%,n=9),检测限为0.2ng·mL^-1;拉米夫定与其右旋对映体可完全分离。结论:本方法灵敏、准确、专属性好,可用于拉米夫定的含量测定、有关物质检查及对映体纯度检查。
Objective:To establish RP - HPLC methods for the determination of lamivudinc and its related substances. Method:Separation of lamivudine and its related substances was performed on a Diamonsil C18 column(200 mm × 4. 6 mm,5 μm). The mobile phase consisted of 0. 025 moL · L^-1 ammonium acetate(pH 3.9 ± 0. 1 ) - methanol(90: 10). The flow rate was 1.0 mL ·min^- 1 and the detection wavelength was 277 nm. Separation of lamivudine enantiomers was performed on a CYCLOBOND I 2000 RSP column(250 mm × 4. 6 mm,5 μm). The mobile phase consisted of 0. 05 moL · L^- 1 ammonium acetate ( pH 3.9 ±0. 1 ) - methanol (95 : 5 ). The flow rate was 0.8 mL · min^-1 and the detection wavelength was 270 nm. Results:Lamivudine was separated completely from impurities. The linear range of lamivudine was 5 - 50 μg · mL^- 1 ( r = 0. 9997 ). The average recovery of lamivudine was 100. 1% with RSD of 0. 69% ( n = 9). The lowest limit of detection was 0. 2 ng · mL^-1. ( - ) - Lamivudine was separated completely from ( + ) -lamivudine. Conclusion:With good sensitivity and selectivity, the method can be applicable for the determination of lamivudine and its related substances.
关 键 词:拉米夫定 含量测定 有关物质 高效
液相色谱法 手性分离 对映体
lamivudine determination related substances HPLC chiral separation enantiomer
分 类 号: R917 [医药、卫生 > 药学 > 药物基础科学]