固相萃取-HPLC法同时测定盐酸帕洛诺司琼注射液中6种杂质

Simultaneous Determination of Six Impurities in Palonosetron Hydrochloride Injections by Solid Phase Extraction-High Performance Liquid Chromatography

目的:固相萃取—高效液相色谱法同时测定盐酸帕洛诺司琼注射液中差向异构体、对映异构体、氮氧杂质等6种杂质的含量。方法:样品经1 mol·L^-1氢氧化钠溶液调节pH,经Agilent Bond Elut C8固相萃取柱(200 mg,3 mL)去除大部分基质干扰,实现净化与富集,再用乙醇洗脱得到富集物。采用USP40盐酸帕洛诺司琼原料药已知杂质测定方法,以Astec CHIROBIOTIC■V(250 mm × 4.6 mm,5 μm)为色谱柱对其进行分离检测。结果:6种杂质在0.2~4.3 μg·mL^-1范围内线性良好,相关系数r≥0.999 5,方法的检测限为0.056~0.065 μg·mL^-1,低、中、高3个浓度的加样回收率为90.60%~105.7%。结论:本方法可用于同时检测盐酸帕洛诺司琼注射液中的6种杂质。

Objective:To develope a simple analytical method of solid phase extraction-high performance liquid chromatography (SPE-HPLC) for the simultaneous determination of six impurities including epimer,enantiomer and N-oxide in palonosetron hydrochloride injections.Methods:The pH of the sample was adjusted by 1 mol·L^-1 sodium hydroxide,then the impurities were enriched by Agilent Bond Elut C8 solid phase extraction (200 mg,3 mL) and eluted with ethanol.The impurities were separated and detected using Astec CHIROBIOTIC■V column (250 mm × 4.6 mm,5 μm) according to the palonosetron hydrochloride monography in USP40.Result:The method showed good linear relationship (r≥0.999 5) in 0.2-4.3 μg·mL^-1 for all the analytes.The limits of detection ranged from 0.056 to 0.065 μg·mL^-1,and the recoveries of all the analytes were between 90.60%-105.7%.Conclusion:The method is suitable for the simultaneous determination of these six impurities in palonosetron hydrochloride injections.