HPLC法测定奥沙利铂杂质B的研究

目的:建立奥沙利铂及其制剂中杂质B(二水二胺环己烷合铂)的HPLC测定方法。方法:采用C18色谱柱;流动相为庚烷磺酸钠溶液(1.36 g磷酸二氢钾和1 g庚烷磺酸钠溶解于1 000 mL水中,用磷酸调pH值至3.0±0.05)-乙腈(83∶17);流量1.0 mL.min-1;检测波长215 nm;柱温40℃。结果:杂质B在11.17～89.36 ng范围内线性关系良好(r=0.999 8),平均回收率为98.7%,RSD为0.5%(n=9),定量限为2.2 ng。结论:所建方法简便、准确,可用于奥沙利铂及其制剂中杂质B的检测。

HPLC Determination of Oxaliplatin Impurity B

Objective. To establish the method for determination of oxaliplatin impurity B （diaquodiaminocyclohexaneplatinum） in oxaliplatin and its preparations. Method： Impurity B was determined by RP-HPLC method using C18 with the column temperature at 40 ℃ and sodium heptanesulphonute solution （ 1.36 g of potassium dihydrogen phosphate and 1 g of sodium heptanesulphunate in 1 000 mL of water, adjust this solution to pH 3.0 ＋ 0. 05 with phosphoric acid ） -acetonitrile （83：17 ） as the mobile phase, the flow rate was 1.0 mL. min^-1 and the detection wavelenth was 215 nm. Results： The linearity was found in the rang of i 1.17-89. 36 ng for impurity B（r =0. 999 8）. The corresponding average recovery was 98.7% with RSD 0. 5% （n =9）. The LOQ was 2.2 ng. Conclusion： The method was simple and convenient. It is suitable for the determination of impurity B in oxaliplatin and its preparations.