劳拉西泮原料及其片剂中有关物质的检查  

HPLC determination of related substances in lorazepam and its tablets

作　　者：程东升[1] 陈蕾[1] 南楠[1] 

机构地区：[1]中国药品生物制品检定所

出　　处：《药物分析杂志》2006年第12期1800-1803,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立 HPLC 法同时测定劳拉西泮原料及片剂中4种有关物质的方法。方法:采用 C_(18)柱(250 mm×4.6 mm,5μm),以0.05 mol·L^(-1)磷酸二氢铵-甲醇-乙腈(35:35:30,用1 mol·L^(-1)磷酸调 pH3.5)为流动相,流速1.0 mL·min^(-1),检测波长240 nm。结果:劳拉西泮峰及各杂质峰均能良好的分离。杂质 B 浓度在0.1964～19.64μg·mL^(-1)范围内与峰面积呈良好的线性关系,回归方程为 Y=51.47317X-3.34831,r=0.9999,最低检测限为3 ng,回收率为100.1%,RSD=0.4%(n=4);杂质 C 浓度在0.202～20.2μg·mL^(-1)范围内与峰面积呈良好的线性关系,回归方程为 Y=36.32533X-4.37263,r=0.9999,最低检测限为0.4 ng,回收率为101.4%,RSD=1.7%(n=4);杂质 D 浓度在0.1992～19.92μg·mL^(-1)范围内与峰面积呈良好的线性关系,回归方程为 Y=70.36881X-2.9103,r=0.9999,最低检测限为0.58 ng,回收率为100.8%,RSD=0.5%(n=4);杂质 E 浓度在0.188～18.8μg·mL^(-1)范围内与峰面积呈良好的线性关系,回归方程为 Y=54.74563X-1.93471,r=0.9997,最低检测限为0.73 ng,回收率为103.1%,RSD=0.7%(n=4)。结论:该方法简便、灵敏、专属性好,可以用于劳拉西泮原料和制剂中有关物质的检查。Objective：To determine four related substances simultaneously in lorazepam and its tablets by HPLC. Methods：The separation was performed on a C18 column （250 mm×4.6mm,5μm）,the mobile phase was composed of 0. 05 mol · L^-1 ammonium dihydrogen orthophosphate methanol- acetonitrile（35： 35：30 ,adjust the solution with 1 mol · L-^ phosphoric acid to a pH of 3.5 ）, the flow rate was 1.0 mL min^-1 and detection at 240 nm. Results ：The separations of lorazepam and its impurities was good. For impurity B ,the calibration curve was linear in the range of 0. 1964-19.64 μg·mL^-1 with correlation coefficient 0. 9999 and the regression equation being Y= 51. 47317X-3. 34831, and the detection limit was 3 ng;The recovery of assay was 100. 1%, and the RSD was 0. 4% （n = 4） . For impurity C, the calibration curve was linear in the range of 0. 202 -20. 2μg·mL^-1 with correlation coefficient 0. 9999 and the regression equation being Y = 36. 32533X - 4. 37263, and the detection limit was 0. 4 ng;The recovery of assay was 101.4% ,and the RSD was 1.7% （n =4）. For impurity D,the calibration curve was linear in the range of 0. 1992 - 19.92 μg·mL^-1 with correlation coefficient 0. 9994 and the regression equation being Y=70. 36881X -2. 9103 ,and the detection limit was 0.58 ng;The recovery of assay was 100. 8% ,and the RSD was 0. 5% （n =4）. For impurity E ,the calibration curve was linear in the range of 0. 188 - 18.8μg·mL^-1 with correlation coefficient 0. 9997 and the regression equation being Y = 54. 74563X - 1. 93471, and the detection limit was 0. 73 ng;The recovery of assay was 103.1% ,and the RSD was 0. 7% （n =4） . Conclusion：The method is simple, sensitive and it is suitable for the determation of the related substances of lorazepam tablets.

关 键 词：劳拉西泮 有关物质 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]