磷酸氟达拉滨的杂质检查及含量测定方法的建立  

Determination of Content and Related Substances of Fludarabine Phosphate

作　　者：付丽娟 陈丽 Fu Lijuan;Chen Li(Wuhan Institute for Drug and Medical Device Control,Wuhan 430075,China)

机构地区：[1]武汉药品医疗器械检验所,武汉430075

出　　处：《中国药师》2019年第5期982-985,共4页China Pharmacist

摘　　要：目的:建立抗癌药磷酸氟达拉滨的杂质检查及含量测定的方法。方法:采用HPLC法,杂质检查采用YMC-Pack ODS-A柱(150 mm×4. 6 mm,4μm),以0. 01 mol·L^(-1)磷酸二氢钾溶液-甲醇(96∶4)为流动相X,以0. 01 mol·L^(-1)磷酸二氢钾溶液-甲醇(80∶20)为流动相Y,分两步骤洗脱,流速为1. 0 ml·min^(-1),260 nm波长检测,柱温为室温,进样量为10"l。含量测定采用Hypersil BDS C_(18)柱(250 mm×4. 6 mm,5"m),以0. 01 mol·L^(-1)磷酸二氢钾溶液-甲醇(96∶4)为流动相,流速为1. 0 ml·min^(-1),检测波长为260 nm,柱温为室温,进样量为20"l。结果:此条件下可分离15种以上磷酸氟达拉滨的杂质。磷酸氟达拉滨在0. 409～122. 700μg·ml^(-1)范围内线性关系良好(r=0. 999 9)。结论:本法操作简便,测定结果准确、重复性好,有利于磷酸氟达拉滨的国产化研究。Objective:To establish a method to determine the content and related substances of fludarabine phosphate.Methods:An HPLC method was used.In the determination of related substances,a YMC-Pack ODS-A column(150 mm×3.9 mm,4μm)was used,the mobile phase X was 0.01 mol·L^-1 monobasic potassium phosphate solution-methanol(96∶4),and the mobile phase Y was0.01 mol·L^-1 monobasic potassium phosphate solution-methanol(80∶20)with two-step elution,the flow rate was 1.0 ml·min-1,the wavelength was 260 nm,the column temperature was room temperature,and the injection volume was 10"l.In the determination of content,a Hypersil BDS C18 column(250 mm×4.6 mm,5"m)was used,the mobile phase was 0.01 mol·L^-1 monobasic potassium phosphate solution-methanol(96∶4),the flow rate was 1.0 ml·min^-1,the detection wavelength was 260 nm,the column temperature was room temperature,and the injection volume was 20"l.Results:More than 15 related substances of fludarabine phosphate were separated.Fludarabine phosphate showed a good linear relationship within the range of 0.409-122.700μg·mL^-1(r=0.999 9).Conclusion:The method is easy to operate and has good accuracy and repeatability.It can provide technical basis for domesticated quality research of anti-cancer medicine fludarabine phosphate.

关 键 词：磷酸氟达拉滨 杂质检查 含量测定 

分 类 号：R927.2[医药卫生—药学]