高效液相色谱法测定硼替佐米中异戊醛含量

HPLC determination isovaleraldehyde content in bortezomib

目的建立高效液相色谱法测定硼替佐米原料药中异戊醛含量。方法硼替佐米中的异戊醛用2,4-二硝基苯肼衍生化,采用Waters symmetry C18色谱柱(250 mm×4.6 mm,5μm),以乙腈(体积分数0.1%甲酸)-水(体积分数0.1%甲酸)为流动相进行线性梯度洗脱,流速为1.0 mL·min^-1,检测波长为364 nm,柱温为30℃。结果异戊醛质量浓度在0.015~2.998 mg·L^-1内与峰面积呈良好线性关系(r=1.0000),平均回收率为101.1%,RSD为1.4%。结论该方法准确灵敏、线性范围宽,可以用于稳定性过程中潜在基因毒性杂质异戊醛的评估。

Objective To establish an HPLC determination isovaleraldehyde content in bortezomib.Methods Isovaleraldehyde in bortezomib was derivatized with 2,4-dinitrophenylhydrazine.Waters symmetry C18(250 mm×4.6 mm,5μm)column was used and the mobile phase was consisted of acetonitrile(including 0.1%formic acid)solution-aqueous(including 0.1%formic acid)with linear gradient elution.The detection wavelength was 364 nm.The flow rate was 1.0 mL·min^-1 and the column temperature was 30℃.Results The linearly related of isovaleraldehyde was 0.015-2.998 mg·L^-1(r=1.0000),the average recovery was 101.1%with a RSD value of 1.4%.Conclusion The established method is accurate,sensitive and simple,and had a wide linear range,can be used for determination isovaleraldehyde content in bortezomibstability test.