高效液相色谱法与紫外光谱法测定索拉非尼原料药含量的比较

目的 分别采用高效液相色谱(HPLC)法与紫外分光光度(UV)法对相同批号的索拉非尼原料药进行含量测定并进行比较.方法 高效液相色谱法中,色谱柱为Inertsil ODS-3柱(250 mm×4.6 mm,5 μm),流动相为乙酸铵缓冲液(50 mmol/L)-乙腈(28:72),检测波长为265 nm,流速为1.0 mL/min,柱温为40℃,进样量为50μL.紫外分光光度法中,索拉非尼原料药样品溶液用甲醇配制,在265 mm波长处进行测定.结果 高效液相色谱法测得索拉非尼进样质量浓度在0.5～40 μg/mL(r=0.99999)范围内与峰面积线性关系良好,平均加样回收率为102.92%,RSD=1.30%(n=9).紫外分光光度法测得索拉非尼进样质量浓度线性范围是0.1～20 μg/mL(r=0.999 9).紫外分光光度法含量测定结果比高效液相色谱法平均高出1.067倍.结论 紫外分光光度法不适用于准确测定索拉非尼原料药的含量.高效液相色谱法的专属性好、稳定性、精密度以及加样回收率都较好,适用于索拉非尼原料药含量的准确测定.

Comparative Study of HPLC and UV Method for the Determination of Sorafenib

Objective To quantify the sorafenib using both HPLC and UV method.Methods HPLC analyses were carried out on an Inertsil ODS-3 column（250 mm×4.6 mm,5 μm）with a mobile phase of ammonium acetate buffer（50 mmol/L）-acetonitrile（28 ∶72）at the flow rate of 1.0 mL/min and a 265 nm detection.The column temperature was 40 ℃and injected sample amount was 50 μL.The UV method with methanol as solvent to prepare a sample has been developed using UV detection at 265 nm.Results HPLC method was validated and found to be linear in the range of 0.5-40 μg/mL（r=0.999 99）;The average recovery was 102.92%with RSD of 1.30%（n=9）.Meanwhile,the linear range of sorafenib was 0.1-20 μg/mL（r=0.999 9）by UV method.The result of UV method was 1.067 times higher than HPLC method.Conclusion The UV method is not appropriate for the determination of sorafenib.The HPLC method with good specificity,stability,precision and recovery rate is appropriate for the determination of sorafenib.