反相液相色谱法同时测定原料药中吉非替尼及其有关物质的含量  

Simultaneous Determination of Gefitinib and Its Related Substances in Raw Material Drugs by Reversed-phase High Performance Liquid Chromatography

作　　者：吴学昊 罗安[1] 叶连宝[1] 陈智[1] 万强[1] 范华均[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：《分析测试学报》2016年第1期35-41,共7页Journal of Instrumental Analysis

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

摘　　要：采用Phenomenex Gemini C18色谱柱,以乙腈-0.15%醋酸铵缓冲液为流动相,紫外检测器检测,通过对流动相组成、缓冲溶液浓度、p H值、检测波长等色谱条件进行研究,建立了同时测定原料药中吉非替尼及其有关物质含量的反相高效液相色谱法。结果表明：以乙腈-0.15%醋酸铵缓冲溶液（p H 8.5）为流动相,流速1.0 m L/min,检测波长255 nm,在40℃柱温下采用梯度洗脱可较好地分离原料药中吉非替尼及其9种有关物质;吉非替尼及其有关物质的质量浓度在0.012 0~4.202μg/m L范围内呈良好线性关系（r〉0.999 0）,检出限为0.001 7~0.094 1μg/m L,平均回收率和相对标准偏差（RSD）分别为99.7%~100.9%和0.06%~0.70%。该法已成功应用于吉非替尼原料药主成分及有关物质的同时测定,且检测灵敏度高,重现性好,结果准确可靠,可作为吉非替尼原料药质量控制的标准。An analytical method for the simultaneous determination of gefitinib and its related sub- stances in raw material drugs was developed by using reversed-phase high performance liquid chroma- tography（ RP -HPLC）. The analysis was carried out on a Phenomenex Gemini C18 column（250 mm x 4.6 mm, 5 μm） with acetonitrile-0. 15% ammonium acetate（pit 8.5） as mobile phase at a flow rate of 1.0 mL/min, detection wavelength of 255 mn and column temperature of 40 ℃ in a gradient elution mode. Under the optimized conditions, gefitinib and its related substances had good hneari- ties in the range of 0. 012 0 - 4. 202 μg/mL （ r 〉 0. 999 0）. Their detection limits were between 0. 001 7 and 0. 094 1 μg/mL. The average recoveries ranged from 99.7% to 100.9% with relative standard deviations （RSDs） of 0. 06% - 0. 70%. The method was applied in the determination of gefitinib and its related substances in raw material drugs with satistactory results, and the method was sensitive, accurate, and was reliable for the quality control of gefitinib in drugs.

关 键 词：反相高效液相色谱法 原料药 吉非替尼 有关物质 质量控制 

分 类 号：O657.32[理学—分析化学]