Yang Guilin, Zhang Nan, Wang Tiance, Zhang Shudong, Xu Rihao, Zhu Zhicheng, Liu Kexiang
The Second Hospital of Jilin University, Changchun, 130041, People's Republic of China; China Meitan General Hospital, Beijing, 100028, People's Republic of China.
Biomed Chromatogr. 2014 Dec;28(12):1789-94. doi: 10.1002/bmc.3222. Epub 2014 May 7.
Vaccarin, a flavonoid glycoside, is considered one of the major active constituents of Vaccaria segetalis. A simple and specific liquid chromatography-tandem mass spectrometric method was developed and validated for quantifying vaccarin in rat plasma following intravenous dosing. Plasma samples were precipitated with methanol and separated on a Venusil-C18 analytical column (2.1 × 50 mm, 5 µm particles) with gradient elution consisting of methanol and 0.1% (v/v) formic acid as the mobile phase. The detection was performed on an Agilent Triple Quad LC/MS with electrospray ionization inlet in the positive multiple reaction monitoring mode. Good linearity was achieved over the concentration range of 12.5-25,000 ng/mL (r(2) > 0.99). Intra- and inter-day precisions were <9.1%, and accuracy ranged from -2.8 to 8.7%. The lower limit of quantification for vaccarin was 12.5 ng/mL, and the analyte was stable under various storage conditions. This validated method was successfully applied to the preliminary pharmacokinetic studies of vaccarin following intravenous administrations of 1.21, 2.41, and 4.82 mg/kg vaccarin in rats.
王不留行黄酮苷是麦蓝菜的主要活性成分之一。建立了一种简单且特异的液相色谱 - 串联质谱法，并对其进行了验证，用于定量大鼠静脉给药后血浆中的王不留行黄酮苷。血浆样品用甲醇沉淀，在Venusil - C18分析柱（2.1×50 mm，5 µm颗粒）上分离，流动相为甲醇和0.1%（v/v）甲酸组成的梯度洗脱液。采用安捷伦三重四极杆液相色谱/质谱仪，在正离子多反应监测模式下，以电喷雾电离进样进行检测。在12.5 - 25,000 ng/mL浓度范围内线性良好（r(2)＞0.99）。日内和日间精密度均＜9.1%，准确度在 - 2.8%至8.7%之间。王不留行黄酮苷的定量下限为12.5 ng/mL，且在各种储存条件下分析物均稳定。该验证方法成功应用于大鼠静脉注射1.21、2.41和4.82 mg/kg王不留行黄酮苷后的初步药代动力学研究。
