HPLC法测定利奈唑胺的有关物质

Determination of the related substances of linezolid by HPLC

目的:建立高效液相色谱法测定利奈唑胺原料药的有关物质。方法:采用InertSustain十八烷基硅烷键合硅胶(4.6 mm×250 mm,5μm)色谱柱,以0.1%三氟乙酸溶液-0.1%三氟乙酸乙腈溶液为流动相,梯度洗脱,流速1.0 mL·min^(-1),柱温30℃,检测波长251 nm。结果:利奈唑胺与10个已知杂质A~K色谱峰之间的分离度良好;各成分检测限0.25~1.27 ng,定量限0.79~2.54 ng,在0.25~1.0μg·mL-1范围内浓度与峰面积线性关系良好(r>0.9990),各杂质平均回收率87.8%~102.9%(n=9)。3批利奈唑胺样品测定结果显示,已知杂质及其他最大单个杂质均小于0.1%,杂质总含量小于0.15%。结论:经方法学验证,本方法灵敏、快速、专属性强、准确度高,可用于利奈唑胺原料药有关物质的测定。

Objective:To establish an HPLC method for determination of related substances in linezolid.Methods:The determination was performed on InertSustain C 18 column(4.6 mm×250 mm,5μm)under gradient elution of 0.1%trifluoroacetic acid solution and 0.1%trifluoroacetic acid acetonitrile solution.The flow rate was 1.0 mL·min^(-1),the column temperature was 30℃and the detection wavelength was 251 nm.Results:The resolutions between linezolid peak and 10 known impurities A-K peaks were good.The limits of detection of linezolid and impurities were 0.25-1.27 ng and the limits of quantitation of them were 0.79-2.54 ng.The calibration curves of linezolid and the known impurities were linear in their respective concentration ranges of 0.25-1.0μg·mL-1(r>0.9990).The average recoveries of impurities were 87.8%-102.9%(n=9)for the above impurities.The determination results of three batches of linezolid samples showed that the known impurities were less than 0.05%,the maximum unknown impurity was less than 0.10%and the total impurities were less than 0.15%.Conclusion:The method was simple,rapid and accurate,and can be used to control the quality of linezolid.