液相色譜-質(zhì)譜法測(cè)定人體血漿中非那雄胺含量
發(fā)布時(shí)間:2018-03-21 09:37
本文選題:液相色譜-質(zhì)譜法 切入點(diǎn):電噴霧離子源 出處:《分析科學(xué)學(xué)報(bào)》2017年06期 論文類(lèi)型:期刊論文
【摘要】:建立了測(cè)定人體血漿中非那雄胺藥物濃度的液相色譜-質(zhì)譜分析方法。色譜柱為Hypersil-Keystone C_(18)柱,流動(dòng)相為乙腈∶水(含0.2%三氯乙酸)=55∶45(V/V),質(zhì)譜選擇電噴霧正離子源(ESI+),選擇離子模式(SIM)監(jiān)測(cè),非那雄胺和內(nèi)標(biāo)卡馬西平質(zhì)荷比分別為m/z373和m/z237。血漿樣品經(jīng)乙腈去蛋白、離心和吹干后,殘?jiān)昧鲃?dòng)相溶解。當(dāng)非那雄胺的濃度在0.5~120ng·mL~(-1)范圍時(shí)線性關(guān)系良好(r=0.999),檢測(cè)限(S/N=3)為0.02ng·mL~(-1);日間和日內(nèi)測(cè)定的精密度(RSD)分別在6.4%~2.2%和5.5%~1.7%之間;加標(biāo)0.5ng·mL~(-1)、40ng·mL~(-1)和80ng·mL~(-1)非那雄胺的平均回收率(n=6)分別為108.5%、101.2%和98.7%。方法快速、準(zhǔn)確和靈敏,已成功用于人血漿中非那雄胺濃度的測(cè)定和人體藥代動(dòng)力學(xué)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.
【作者單位】: 衢州學(xué)院化學(xué)與材料工程學(xué)院;常德市食品藥品檢驗(yàn)所;
【基金】:浙江省自然科學(xué)基金(No.LY15B050008)
【分類(lèi)號(hào)】:O657.63;R969
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