目的 建立UPLC-MS/MS測(cè)定比格犬血漿中的五味子醇甲血藥濃度分析方法。方法 采用ACQUITY UPLC^® BEH C₁₈色譜柱（50 mm×2.1 mm，1.7 μm），流動(dòng)相為0.1%乙酸水-甲醇梯度洗脫，體積流量為0.4 mL/min。柱溫40℃，進(jìn)樣量5 μL。采用電噴霧（ESI）正離子模式進(jìn)行多反應(yīng)（MRM）監(jiān)測(cè)，五味子醇甲和利伐沙班（內(nèi)標(biāo)）的定量離子對(duì)分別為m/z 433.20→384.30、437.19→145.13。結(jié)果 五味子醇甲在0.2～100 ng/mL線性關(guān)系良好（r=0.999 6），最低定量限為0.2 ng/mL，批內(nèi)、批間精密度分別為2.04%～7.62%、3.72%～8.29%；基質(zhì)效應(yīng)及提取回收率分別為95.7%～103%、81.2%～106%；穩(wěn)定性結(jié)果均符合生物樣品檢測(cè)指導(dǎo)原則。結(jié)論 建立的UPLC-MS/MS方法快速、簡單、靈敏度高，能滿足五味子醇甲血藥濃度測(cè)定及其藥動(dòng)學(xué)研究。

Objective To establish UPLC-MS/MS method for determination of schisandrin in plasma of Beagle dogs. Methods The determination was carried out on ACQUITY UPLC^® BEH C₁₈ column (50 mm×2.1 mm, 1.7 μm). The mobile phase consisted of 0.1% acetic acid water-methanol with gradient elution at a flow rate of 0.4 mL/min. The column temperature was set at 40 ℃, and the injection volume was 5 μL. Electrospray positive ion mode was used for multi reaction monitoring, the quantitative ions of schisandrin and rivaroxaban (IS) were m/z 433.20→384.30 and 437.19→145.13, respectively. Results Schisandrin had good linearity in the ranges of 0.2 — 100 ng/mL (r=0.999 6). The minimum quantitative limit was 0.2 ng/mL, the intra and inter-day precision were 2.04% — 7.62% and 3.72% — 8.29%, respectively. The matrix effect and the recovery of extraction in the low, medium and high concentration were 95.7% — 103% and 81.2% — 106%, respectively. The results of stability accorded with the guiding principles of biological sample detection. Conclution The UPLC-MS/MS method is rapid, simple and sensitive, and can be used for the determination of schisandrin A in blood and its pharmacokinetics.

R969.1

國家科技重大專項(xiàng)（2015ZX09501004）