HPLC-DAD法测定甲磺酸伊马替尼含量及有关物质  

HPLC- DAD determination of imatinibmesylate content and its related substances

作　　者：傅小勤[1] 陈保来[1] 仲艳[1] 李家春[1] 郭庆明[1] 肖伟[1] 

机构地区：[1]江苏康缘药业股份有限公司,连云港222000

出　　处：《药物分析杂志》2013年第12期2135-2140,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的：建立HPLC-DAD法测定甲磺酸伊马替尼原料药含量及有关物质。方法：采用Waters X-Bridge C18（250 mm×4.6 mm，5 μm）色谱柱，甲醇-三乙胺溶液（用磷酸调pH至8.0）为流动相，梯度洗脱，流速为1.0 mL·min-1，检测波长为268 nm，柱温30 ℃，进样体积为10 μL。结果：此色谱条件下，各组分之间分离度均大于2.0，线性范围9.09~90.92 μg·mL-1 （r=0.9998），检测限为0.3 ng。结论：该方法简便、准确、灵敏度高、重复性好，可避免使用辛烷基磺酸钠离子对试剂对色谱柱寿命的影响。Objective： To establish an HPLC-DAD method for content determination of imatinibmesylate and its related substances. Methods： The separation was performed on a Waters X-Bridge C18（250 mm×4.6 mm,5 μm）column;The mobile phase was methanol-0.5% triethylamine aqueous solution（adjusted to pH 8.0 with phosphoric acid）by gradient elution at a flow rate of 1.0 mL·min-1;The detection wavelength was 268 nm;The column temperature was 30 ℃;The injection volume was 10 μL. Results： The imatinibmesylate and related substances could be separated,and the resolution was more than 2.0.The linear range of imatinibmesylate was 9.09-90.92 μg·mL-1（r=0.9998）,the detection limit was 0.3 ng. Conclusion： The established method is simple,accurate and sensitive;it also avoids the use of 1-octanesulfonic acid sodium salt which affects the longevity of both reagents and columns.

关 键 词：甲磺酸伊马替尼 原料药含量 杂质测定 梯度洗脱 液质联用 HPLC—DAD 

分 类 号：R917[医药卫生—药物分析学]