HPLC法测定普乐沙福原料药的有关物质

Determination of the Related Substances in Plerixafor by HPLC

目的:建立普乐沙福原料药有关物质的反相离子对高效液相色谱法。方法:采用离子对反相高效液相色谱法分析,以对照品外标法定性和定量。采用沃特世Xbridge C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为pH2.0庚烷磺酸钠-乙腈(80∶20),流速1.0 ml·min^(-1),检测波长210 nm,柱温35℃,进样量10μl。结果:普乐沙福与相邻杂质之间的分离度均大于1.5;有关物质1、2、3的定量限分别为21、35、26 ng,且在各自的线性范围内线性关系良好(r≥0.999 0);平均回收率分别为99.7%,100.3%,101.2%,RSD分别为1.1%,0.8%,1.7%(n=9)。结论:该方法专属性强、准确度高,适用于普乐沙福原料药的质量控制。

Objective： To develop a novel method for the determination of the related substances in plerixafor. Methods： A re- versed-phase ion-paired HPLC method was applied in the qualitative and quantitative determination of plerixafor by an external standard method. The method was performed on a Waters Xbridge C18 column （250 mm× 4.6 mm, 5 μm） , the mobile phase consisted of 1- heptancsulfonic acid sodium salt buffer （pH 2.0） and aeetonitrile with the ratio of 80：20 （v/v）, the flow rate was 1.0 ml .min-1 , the detection wavelength was 210 nm, the column temperature was 35℃ , and the injection volume was 10 ixl. Results： The degrada- tion products were well separated from the main peak, the LOQ （limits of quantitative） of the related substance 1,2 and 3 respectively was 21 ng, 35 ng and 26 ng with good linearity within respective linear range（ r≥0. 999 0） , the average recovery was 99.7%, 100.3 % and 101.2%, and RSD was 1.1%, 0.8% and 1.7% , respectively （n = 9）. Conclusion： The method is specific and accu- rate, which can be used for the quality control of plerixafor.