RP-HPLC法同时测定多沙唑嗪及其中间体  

Simutaneously Determination of Doxazosin and Its Intermediates by RP-HPLC

作　　者：陈志琼[1,2] 熊正平[1] 余瑜[2] 

机构地区：[1]重庆医科大学药物分析教研室,重庆400016 [2]重庆医科大学药物化学与生物材料研究室,重庆400016

出　　处：《精细化工》2009年第3期284-287,共4页Fine Chemicals

基　　金：国家自然科学基金资助项目(30371632);重庆市科委资助项目(2002-14-025);重庆市教委资助项目(2002-18-004);重庆医科大学资助项目(XB200332)~~

摘　　要：多沙唑嗪通常由中间体BCP和ACQ合成，为考察产品质量，有必要建立多沙唑嗪及其中间体的测定方法。该文建立并优化了反相高效液相色谱法（RP—HPLC）同时测定多沙唑嗪及其中间体。结果表明，以C18柱（4．6mm×250mm）为色谱柱，流动相组成V（CH3OH）：V[c（KH2PO4）=0．02mol／L，pH=3．0]=70：30，流速0．6mL／min，检测波长246nm，多沙唑嗪与BCP、ACQ可达到基线分离，分离度大于2．0。各物质在1-20mg／L内的色谱峰面积与质量浓度之间线性关系良好（r〉0．999），该方法的准确度（回收率〉99％）和精密度（RSD〈4％）高，操作简便快速，可望用于多沙唑嗪产品质量研究和控制。Doxazosin is usually synthesized by 1-（ 1,4-benzodioxane-2-carbonyl） piperazine （BCP） and 4-amino-2-chloro-6,7-dimethoxyquinazoline（ACQ）. It is very important to assay the content of such two intermediates in doxazosin in order to guarantee the product quality. A reversed phase highperformance liquid chromatographic （ RP - HPLC） method for the simutaneous separation of doxazosin and its intermediates has been developed and optimized. The results showed that the doxazosin and its intermediates could be separated on the C18 column with a mobile phase consisting of methanol and 0. 02 mol/L aqueous potassium dihydrogen phosphate solution（70：30,pH =3.0） at a flow rate of 0. 6 mL/min and the wavelength for detection was set at 246 nm. The results showed that two intermediates and doxazosin were separated with the baseline method under the optimum conditions （ R 〉 2.0 ）. Through the concentration range of 1 -20 mg/L, the linearity is valid between the peak area and the chemicals＇ mass concentration （the regression coefficient is above 0. 999 ）. Both the accuracy and precision of this method are Kood, so it can be applied to the quality study and contro of doxazosin.

关 键 词：多沙唑嗪 1-(1 4-苯并二嗯烷-2-羰基)哌嗪 4-氨基-2-氯-6 7-二甲氧基喹唑啉 HPLC 医药与日化原料 

分 类 号：R927.2[医药卫生—药学]