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建立测定人血浆中丹参酮IIA含量的LC-MS/MS方法。取正常人血浆200μL,然后加入200ng/mL隐丹参酮溶液(内标)20μL,加入580μL乙腈沉淀,离心10min(15000rpm)后,取上清液吹干溶剂后,用10%乙腈400μL溶解,取5μL进行LC-MS/MS测定。LC条件:采用ASBC_(18)柱(2.1×50mm,5μm),流动相:乙腈-水梯度洗脱,流速:0.5mL/min。质谱条件:ESI电离源,正离子模式,多反应监测(MRM)方式,用于定量分析的离子对分别为m/z 295.1→m/z 249.2(丹参酮ⅡA)和n/z 297.2→221.1(内标,隐丹参酮)。该方法丹参酮IIA的线性范围为0.4～800ng/mL,最低检测限为0.2ng/mL。本方法操作简便、快速、结果准确、可用于该药物的含量测定,同时也可为临床药代动力学研究提供参考。
A LC-MS / MS method for the determination of tanshinone IIA in human plasma was established. Take normal human plasma 200μL, then add 200ng / mL cryptotanshinone solution (internal standard) 20μL, add 580μL acetonitrile precipitation, centrifuged 10min (15000rpm), the supernatant was evaporated to dryness, dissolved in 400μL 10% acetonitrile, LC-MS / MS measurement was performed. LC conditions: ASBC_ (18) column (2.1 × 50 mm, 5 μm), mobile phase: acetonitrile-water gradient, flow rate: 0.5 mL / min. Mass spectrometry conditions: ESI ionization source, positive ion mode, multiple reaction monitoring (MRM) mode, and the ion pairs for quantitative analysis were m / z 295.1 → m / z 249.2 (tanshinone IIA) and n / z 297.2 → 221.1 Standard, cryptotanshinone). This method tanshinone IIA linear range of 0.4 ~ 800ng / mL, the minimum detection limit of 0.2ng / mL. The method is simple, rapid and accurate, and can be used for the determination of the drug content, and also provides a reference for clinical pharmacokinetic studies.