摘要
目的建立测定激素性股骨头坏死患者血浆中甲泼尼龙质量浓度的超高效液相色谱(UPLC)法。方法色谱柱为Waters Acquity UPLC BSH C18柱(50 mm×2.1 mm,1.7μm),流动相为乙腈-水(29∶71,V/V),流速为0.3 m L/min,检测波长为242 nm,柱温为30℃,进样量为1μL。结果患者血浆中甲泼尼龙与血浆内源性物质分离良好,甲泼尼龙及内标(地塞米松)保留时间分别为3.69,4.28 min;甲泼尼龙血药浓度在0.125~3.0μg/m L范围内与峰面积线性关系良好;检测限和定量限分别为0.05,0.125μg/m L;日间、日内精密度的RSD均不大于4.30%(n=5);室温放置8 h、反复冻融3次、冷冻7 d的稳定性试验的RSD均不大于4.00%(n=5);平均方法回收率为95.93%,RSD为1.40%(n=5);平均提取回收率为75.99%,RSD为2.57%(n=5)。结论所建立的UPLC法运行时间短,待测物与血浆内源性物质分离度好,灵敏度高,可用于测定激素性股骨头坏死患者血浆中甲泼尼龙质量浓度。
Objective To establish an ultra high-performance liquid chromatography(UPLC)method for the determination of the plasma concentration of methylprednisolone in patients with steroid-induced femoral head necrosis.Methods The chromatographic column was Waters Acquity UPLC BSH C18 column(50 mm×2.1 mm,1.7μm),the mobile phase was acetonitrile-water(29∶71,V/V),the flow rate was 0.3 m L/min,the detection wavelength was 242 nm,the column temperature was 30°C,and the injection volume was 1μL.Results Methylprednisolone in plasma was well separated from plasma endogenous substances.The retention time of methylprednisolone and internal standard(dexamethasone)was 3.69 and 4.28 min,respectively.The linear range of methylprednisolone was 0.125-3.0μg/m L,the limit of detection(LOD)and limit of quantitation(LOQ)of methylprednisolone were 0.05 and 0.125μg/m L,respectively.The RSDs of intra-day and inter-day precision tests were not higher than 4.30%(n=5).The RSDs of the stability test after 8 h at room temperature,three repeated freeze-thaw cycles and 7-day freezing were not higher than 4.00%(n=5).The average recovery of the method was 95.93%with RSD of 1.40%(n=5).The average recovery of extraction was 75.99%with RSD of 2.57%(n=5).Conclusion The established UPLC method has the advantages of short running time,good separation and high sensitivity,which can be used for the determination of the plasma concentration of methylprednisolone in patients with steroid-induced femoral head necrosis.
作者
张丽藏
张霞
刘剑
张志清
董维冲
范欣欣
ZHANG Licang;ZHANG Xia;LIU Jian;ZHANG Zhiqing;DONG Weichong;FAN Xinxin(Department of Pharmacy,The Second Hospital of Hebei Medical University,Shijiazhuang,Hebei,China 050000;School of Pharmacy,Hebei Medical University,Shijiazhuang,Hebei,China 050017)
出处
《中国药业》
CAS
2021年第16期65-68,共4页
China Pharmaceuticals
基金
河北省中医药管理局科研计划项目[2021146]。
