Ye X D, Ouyang H, Zhong L Y, Li T E, Rao X Y, Feng Y L, Yang W L
Jiangxi University of Traditional Chinese Medicine, Nanchang, China.
State Key Laboratory of Innovative Drug and Efficient Energy-Saving Pharmaceutical Equipment, Nanchang, China.
Genet Mol Res. 2016 Jun 24;15(2):gmr8786. doi: 10.4238/gmr.15028786.
A simple, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of auraptene, a constituent isolated from Fructus aurantii with potential to combat Alzheimer's disease, in rat plasma. Rat plasma samples were pretreated by protein precipitation with methanol. The analytes were separated by a Waters Sun Fire C18 column (50 mm x 2 mm, 5 μm) and eluted with 1:1000 methanol and formic acid/water (v/v) mobile phase with a flow rate of 0.5 mL/min. Multiple reaction monitoring was used to monitor the transition of the deprotonated auraptene molecule with an m/z of 299.3 M+H, to the product ion with an m/z of 162.9 M+H. Progesterone, with an m/z of 315.2→ 96.9 was used as an internal standard. The limits of detection and of quantification of auraptene in the rat plasma were 1 and 5 ng/mL, respectively. The method was linear in the concentration range of 20- 2000 ng/mL with coefficient correlation of 0.9956. After auraptene (100 mg/kg, p.o.) administration, the maximum plasma concentration and the time taken to reach maximum concentration were 1719.5 ± 384.3 g/mL and 108.0 ± 25.3 min, respectively. The elimination half-life was 108.0 ± 25.3 for auraptene (100 mg/kg, p.o.) and 3.0 ± 0 min for auraptene (2 mg/kg, i.v.). The oral bioavailability was about 8.5%.
建立了一种简单、灵敏且特异的液相色谱-串联质谱法，并对其进行了验证，用于测定大鼠血浆中奥洛普特（一种从枳实中分离出的具有对抗阿尔茨海默病潜力的成分）。大鼠血浆样品用甲醇进行蛋白沉淀预处理。分析物通过沃特世Sun Fire C18柱（50 mm×2 mm，5μm）分离，以1:1000甲醇和甲酸/水（v/v）的流动相洗脱，流速为0.5 mL/min。采用多反应监测模式监测去质子化的奥洛普特分子（m/z为299.3 M+H）向m/z为162.9 M+H的产物离子的跃迁。以m/z为315.2→96.9的孕酮作为内标。大鼠血浆中奥洛普特的检测限和定量限分别为1和5 ng/mL。该方法在20 - 2000 ng/mL的浓度范围内呈线性，相关系数为0.9956。口服给予奥洛普特（100 mg/kg）后，血浆最大浓度和达到最大浓度的时间分别为1719.5±384.3 ng/mL和108.0±25.3 min。奥洛普特（100 mg/kg，口服）的消除半衰期为108.0±25.3 min，奥洛普特（2 mg/kg，静脉注射）的消除半衰期为3.0±0 min。口服生物利用度约为8.5%。
