液相色谱-质谱法测定人体血浆中非那雄胺含量

发布时间：2018-03-21 09:37

本文选题：液相色谱-质谱法　切入点：电喷雾离子源　出处：《分析科学学报》2017年06期 　论文类型：期刊论文

【摘要】：建立了测定人体血浆中非那雄胺药物浓度的液相色谱-质谱分析方法。色谱柱为Hypersil-Keystone C_(18)柱,流动相为乙腈∶水(含0.2%三氯乙酸)=55∶45(V/V),质谱选择电喷雾正离子源(ESI+),选择离子模式(SIM)监测,非那雄胺和内标卡马西平质荷比分别为m/z373和m/z237。血浆样品经乙腈去蛋白、离心和吹干后,残渣用流动相溶解。当非那雄胺的浓度在0.5~120ng·mL~(-1)范围时线性关系良好(r=0.999),检测限(S/N=3)为0.02ng·mL~(-1);日间和日内测定的精密度(RSD)分别在6.4%~2.2%和5.5%~1.7%之间;加标0.5ng·mL~(-1)、40ng·mL~(-1)和80ng·mL~(-1)非那雄胺的平均回收率(n=6)分别为108.5%、101.2%和98.7%。方法快速、准确和灵敏,已成功用于人血浆中非那雄胺浓度的测定和人体药代动力学研究。
[Abstract]:A liquid chromatography-mass spectrometry (LC-MS) method was established for the determination of the concentration of vanasteride in human plasma. The mobile phase consisted of acetonitrile: water (containing 0.2% trichloroacetate (55: 45V / V), mass spectrometry selected electrospray positive ion source (ESI), selective ion mode (Simm)) monitoring, phenasteride and internal standard carbamazepine mass charge ratios were m/ z 373 and m / z 237 respectively. Plasma samples were removed by acetonitrile, centrifuged and blown dry. The residue was dissolved in mobile phase. When the concentration of fenasteride was in the range of 0.5 ~ 120ng 路mL ~ (-1), the linear relationship was 0.999N, the detection limit was 0.02ng 路mL ~ (-1) ~ (-1), and the precision RSDs of day and day were between 6.42% and 5.5 ~ 1.7%, respectively. The average recoveries of 0. 5 ng 路mL ~ (-1) and 80 ng 路mL ~ (-1) finasteride were 108.52% and 98.7%, respectively. The method was rapid, accurate and sensitive. The method has been successfully applied to the determination of the concentration of central androstamine in human plasma and pharmacokinetic study in human body.
【作者单位】：衢州学院化学与材料工程学院;常德市食品药品检验所;
【基金】：浙江省自然科学基金(No.LY15B050008)
【分类号】：O657.63;R969

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