吉非替尼片含量测定方法考察  

Determination of Gefitinib in Tablets

作　　者：叶国健[1] 秦凌浩[1] 胡巧红[1] 

机构地区：[1]广东药学院药科学院,广东广州510006

出　　处：《广东化工》2016年第5期91-92,共2页Guangdong Chemical Industry

基　　金：广东省战略性新兴产业核心技术攻关计划项目(编号2012A080800012)

摘　　要：目的：建立一种测定吉非替尼片中药物含量的方法。方法：采用高效液相色谱法,色谱柱为Spolar C18（5μm,150 mm×4.6 mm）,检测波长为247 nm,流动相为乙腈-乙酸铵溶液,流速1 ml/min。首先通过考察流动相中乙酸铵浓度、乙腈与乙酸铵溶液的比例筛选得到合适的色谱条件,并对该色谱系统进行验证。然后对含量测定样品制备的溶剂组成进行考察,确定合适的样品制备溶剂。结果：流动相为乙腈：0.6%乙酸铵溶液（40∶60,v/v）,样品溶剂为含0.1%（v/v）乙酸的乙腈-水（40∶60,v/v）。该色谱条件下,药物在浓度为10～150μg/ml的范围内线性良好（r=0.9999）;回收率平均值为99.84%,RSD值为0.15%;精密度良好,RSD值为0.41%（n=6）;8小时内样品稳定性良好,RSD值为1.01%。结论：建立的HPLC含量测定方法稳定可靠,适于测定吉非替尼片中药物的含量。Objective To establish an HPLC method to determine gefitinih in tablets. Methods Spolar C18 column （5 μm, 150mm×4.6 mm） was used in the HPLC system. The detection wavelength was 247 nm. The mobile phase was the mixture of acetonitrile and ammonium acetate solution, and the flow rate was 1 ml/min. By investigating the concentration of ammonium acetate and the ratio of mobile phase, chromatographic condition was validated. Then the solvent of sample was confirmed by study the concentration of acetic acid. Results The mobile phase was consist of acetonitrile-0.6 % ammonium acetate solution （40 ; 60, v/v）, and the solvent was acetonitrile-water （40 ： 60, v/v） containing 0.1% （v/v） acetic acid. The calibration curve had a good linearity in the range of 10-150 μg/ml （r=0.9999）. The recovery of gefitinib was 99.84 % （RSD=0.15 %）. The precision was also good with RSD of 0.41% （n=6）, and the sample was stable in 8 hours with RSD of 1.01%. Conclusion The HPLC method is reliable. It is suitable to be used for the determination of gefitinib in tablets.

关 键 词：吉非替尼 含量 高效液相色谱法 

分 类 号：O65[理学—分析化学]