Faculty of Functional Food and Wine, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang 110016, China.
Faculty of Traditional Chinese Materia Medica, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang 110016, China.
Molecules. 2018 Jul 12;23(7):1702. doi: 10.3390/molecules23071702.
A simple and rapid ultra-performance liquid chromatography⁻tandem mass spectrometry (UPLC⁻MS/MS) coupled with a one-step liquid-liquid extraction method has been developed and validated for the simultaneous determination of two flavonoids (chrysin, tectochrysin) from fruits extract in rat plasma. Plasma samples were extracted with diethyl ether and separated on an ACQUITY UPLC BEH C column (100 mm × 2.1 mm, 1.7 μm) using gradient elution consisting of 0.1% formic acid in water (A) and methanol (B). The multiple reaction monitoring (MRM) mode with electrospray ionization in the positive ion mode was used for detection. The linear range was 0.1 ng/mL to 50 ng/mL for chrysin and tectochrysin, respectively. The accuracy (relative error, RE%) ranged from -8.8% to 7.5% and the intra-day and inter-day precision were within 15% and had a mean extraction recovery rate of 80.3% to 86.7%. The validated method was applied to a comparative pharmacokinetic study after oral administration of fruit ethanol extract between normal rats and dementia rats. The area under the curve (AUC) and peak plasma concentration () of the two constituents were remarkably increased in dementia rats than in normal rats.
建立并验证了一种简单快速的超高效液相色谱-串联质谱(UPLC-MS/MS)法,用于同时测定大鼠血浆中两种黄酮类化合物(白杨素、桑色素)的含量。采用乙醚一步液液萃取法提取血浆样品,在 ACQUITY UPLC BEH C 柱(100mm×2.1mm,1.7μm)上以含 0.1%甲酸的水(A)和甲醇(B)为流动相进行梯度洗脱。采用正离子模式电喷雾电离多反应监测(MRM)模式进行检测。白杨素和桑色素的线性范围分别为 0.1ng/mL 至 50ng/mL。准确度(相对误差,RE%)在-8.8%至 7.5%之间,日内和日间精密度均在 15%以内,平均提取回收率为 80.3%至 86.7%。该方法已应用于正常大鼠和痴呆大鼠灌胃果乙醇提取物后的比较药代动力学研究。与正常大鼠相比,痴呆大鼠中两种成分的曲线下面积(AUC)和血浆峰浓度()显著增加。