甲苯磺酸索拉非尼原料药HPLC含量测定的方法学研究  

Validation of HPLC method for the determination of sorafenib tosylate

作　　者：毛依群 何永梅 MAO Yiqun HE Yongmei(Shanghai Pharmaceutical School ,Shanghai 200135, China)

机构地区：[1]上海市医药学校,200135 [2]南京斯贝源医药科技有限公司,南京市210000

出　　处：《临床合理用药杂志》2017年第10期7-9,共3页Chinese Journal of Clinical Rational Drug Use

摘　　要：目的建立了一种能简单准确地测定甲苯磺酸索拉非尼原料药含量的高效液相色谱法(HPLC),并对该方法进行了方法学验证。方法采用HPLC梯度洗脱对甲苯磺酸索拉非尼原料药进行含量测定,色谱柱为Inertsil ODS SP(4.6×150 mm,5μm),流动相A为10 m M磷酸二氢钾缓冲溶液(pH=3.0);流动相B为乙腈—乙醇(1∶1),检测波长为235 nm,柱温为40℃,流速为1.0 ml/min。在实验中通过对系统适用性、精密度、专属性、标准曲线与线性、回收率、重复性等的测定确保方法的准确性。结果索拉非尼与相邻杂质峰之间的分离度良好;索拉非尼在0.02403~0.03605 mg/ml的浓度范围内,线性关系良好;平均回收率为100.20%,RSD为1.05%。结论该方法专属性强,重复性好,准确度高,可用于甲苯磺酸索拉非尼原料药含量的测定。Objective A simple,precise and rapid HPLC（ high performance liquid chromatography） method was developed and validated for sorafenib tosylate API. Methods The content of sorafenib tosylate API was determinated by HPLC gradient elution. The column was Inertsil ODS SP（ 4. 6 × 150 mm,5 μm） and the mobile phase A was 10 m M potassium dihydrogen phosphate buffer solution（ p H = 3. 0）; and mobile phase B was acetonitrile-ethanol（ 1 ∶ 1）. The detection wavelength was 235 nm,the column temperature was 40 ℃ and the flow rate was 1. 0 ml/min. The contents included system applicability,precision,specificity,standard curve and linearity,accuracy were researched to ensure the accuracy of the method. Results The total separation was achieved between sorafenib and adjacent impurities. The standard curve was linear during the range of0. 02403 - 0. 03605 mg/ml. The average recovery was 100. 20%,RSD = 1. 05%. Conclusion The method is highly specific,reproducible and accurate. It can be used for determination of sorafenib tosylate API concentration.

关 键 词：高效液相色谱法 甲苯磺酸索拉非尼 含量测定 

分 类 号：R927.2[医药卫生—药学] O657.72[理学—分析化学]