摘要
目的建立和验证UPLC-MS/MS测定人血浆中长春西汀和阿朴长春胺酸的方法,并用于临床样品检测。方法以长春西汀-d5、阿朴长春胺酸-d4为内标,人血浆样品经蛋白沉淀法沉淀处理,色谱柱为Waters ACQUITY UPLC?BEH C18(2.1 mm×50 mm,1.7μm),流动相为乙腈-水(含0.05%甲酸),梯度洗脱,流速0.35 mL·min^(-1);电喷雾离子化源正离子监测模式。结果长春西汀和阿朴长春胺酸线性范围分别为0.04~20.0 ng·mL^(-1)(r=0.9997)、0.50~250 ng·mL^(-1)(r=0.9996),检测限分别为0.01,0.10 ng·mL^(-1),待测物与内标提取回收率均为94.81%~105.0%,基质效应为94.51%~105.0%,RSD均<5%;批内、批间精密度RSD均<10%。结论本法特异性强、快速、准确,重复性好,适用于长春西汀临床生物样品检测及生物等效性研究。
OBJECTIVE To establish and validate a UPLC-MS/MS for the determination of vinpocetine and apovincaminic acid in human plasma and apply to the determination of clinical samples.METHODS Vinpocetine-d5 and apovincaminic acid-d4 were used as internal standards.Human plasma samples were prepared with acetonitrile to precipitate to protein.The chromatographic column was Waters ACQUITY UPLC?BEH C18(2.1 mm×50 mm,1.7μm),the mobile phase was acetonitrile-water(containing 0.05%formic acid).Gradient elution with a flow rate of 0.35 mL·min-1.Mass spectrometry conditions:Electrospray ionization source(ESI),positive ion detection mode.RESULTS The linear range were0.04-20.0 ng·mL^(-1)(r=0.9997)for vinpocetine and 0.50-250 ng·mL^(-1)(r=0.9996)for apovincaminic acid,and the limit of quantification were 0.01,0.10 ng·mL^(-1),respectively.The recoveries of test sample and internal standard were in the range of94.81%-105.0%,and the matrix effect were 94.51%-105.0%,RSDs were<5%.The RSDs of intra-and inter-batch precision were all<10%.CONCLUSION The method is specific,rapid,accurate and reproducible.Therefore,it is suitable for the determination of vinpocetine concentration in plasma and can applied to its bioequivalence study.
作者
张林琪
苏文俏
郭建军
游宇
胡林
周文
ZHANG Linqi;SU Wenqiao;GUO Jianjun;YOU Yu;HU Lin;ZHOU Wen(EverPro Medical Co.,Ltd.,Changsha 410205,China)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2023年第4期489-493,共5页
Chinese Journal of Modern Applied Pharmacy