梯度洗脱反相高效液相色谱法测定拉呋替丁纯度及含量  

Purity and Content Determination of Lafutidine by Gradient RP-HPLC

作　　者：娄艳红[1] 李小青[1] 谢剑炜[1] 

机构地区：[1]军事医学科学院毒物药物研究所,北京100850

出　　处：《药物分析杂志》2005年第7期831-834,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立梯度洗脱反相高效液相色谱法测定拉呋替丁纯度及含量,并对其未知杂质进行研究。方法:采用梯度洗脱方法,色谱柱为大连依利特科学仪器有限公司Hypersil ODS C18柱(250 mm ×4.6 mm,5μm)。流动相A:0.01 mol.L-1磷酸二氢钾溶液,0.1%三乙胺,用磷酸调节pH 5.0;流动相B:乙腈。梯度洗脱条件:0-12 min,A-B(80:20);12-20min,A-B(40 :60);20-25min,A-B(80:20)。检测波长:220 nm;流速:1.0 mL·min-1。结果:拉呋替丁在0.01-0.50 mg·mL-1范围内线性良好,回归方程为Y=57.72X-21.31(n=5),r=0.9999。结论:建立的液相色谱法可完全分离拉呋替丁、各中间体、副产物等,该方法准确、灵敏、简便,专属性好。经液相色谱、质谱等鉴定确证,本品主要未知杂质为二氢拉呋替丁。Objective:An RP-HPLC method was established for the purity test and assay of lafutidine(LA),and unknown impurity of lafutidine was also studied. Methods:The gradient elution was used with a flow rate of 1.0mL ·min and UV detection at 220 nm. The column was Hypersil ODS column (250mm×4.6mm,5μm) purchased from Dalian Elite Scientific Instrument Co. Ltd. Mobile phase A:0.01 mol·L-1 potassium dihydrogen phosphate buffer,0.1% triethyl amine,adjusting pH 5.0 using phosphoric acid; Mobile phase B:acetonitrile. Condition of the gradient elution:0-12 min, A-B(80=20);12-20 min, A - B(40:60) ; 20-25 min, A- B(80:20). Results:A linear range of lafutidine was 0. 01 -0. 50 mg·mL-1, regression equation was Y =57.72X-21.31(n= 5),r=0.9999. Conclusion:Good chromatographic separation of lafutidine and its intermediate products and by -products was obtained. The accurate,sensitive, simple and selective method is applied to determine the purity of lafutidine.The main impurity N-[4-(4-piperidylmethyl-pyridyl-2-oxy) -butyl] -2-(2-furfuryl) sulfi-nylacetamide(2H-LA) was identified by HPLC and MS technique.

关 键 词：反相高效液相色谱法 拉呋替丁 梯度洗脱 含量 纯度 测定 未知杂质 磷酸二氢钾 科学仪器 C18柱 洗脱条件 检测波长 回归方程 流动相 色谱柱 ODS 三乙胺 中间体 副产物 专属性 

分 类 号：R927.2[医药卫生—药学] R975.6