Chen Jianbo, Chen Lixue, Li Meijia, Sun Yinshi
Institute of Special Wild Economic Animals and Plants, Chinese Academy of Agriculture Sciences, Changchun, People's Republic of China.
College of Traditional Chinese Medicinal Material, Jilin Agricultural University, Changchun, Jilin, People's Republic of China.
Biomed Chromatogr. 2019 Jan;33(1):e4377. doi: 10.1002/bmc.4377. Epub 2018 Oct 9.
In this study, a sensitive hydrophilic interaction liquid chromatography (HILIC) method was developed to determine pseudojervine (PJV), veratrosine (VTS), jervine (JV), veratramine (VTM), veramarine (VA) and veratroylzygadenine (VTG) in rat plasma. Separations were carried out using LC-MS/MS with a Chrom Matrix HP amide column (5 m, 10 cm × 3.0 mm i.d.). The mobile phases were (A) 0.01 mm formic acid and (B) acetonitrile. Good linearity was found for all analytes (R > 0.995) in the concentration range from 5 to 1000 μg/L with LLOQ at 5 μg/L for VTM and VTS; and from 1 to 1000 μg/L with LLOQ at 1 μg/L for PJV, JV, VA and VTG. Accuracy of the assay varied from 90.5 to 108.1%. The extraction recovery and matrix effect of six analytes ranged from 72.2 to 95.5% and from 79.2 to 98.4%. According to the stability test, six analytes in rat plasma were stable during the analysis process. On the basis of validation of the assay, the pharmacokinetics of the six steroid alkaloids were investigated after oral administration of Lilu extracts to rats.
在本研究中，开发了一种灵敏的亲水作用液相色谱（HILIC）方法，用于测定大鼠血浆中的伪杰尔文（PJV）、藜芦胺（VTS）、杰尔文（JV）、藜芦胺（VTM）、藜芦碱（VA）和藜芦酰棋盘花碱（VTG）。使用配备Chrom Matrix HP酰胺柱（5μm，10cm×3.0mm内径）的LC-MS/MS进行分离。流动相为（A）0.01mm甲酸和（B）乙腈。所有分析物在5至1000μg/L的浓度范围内均具有良好的线性（R>0.995），VTM和VTS的定量下限（LLOQ）为5μg/L；PJV、JV、VA和VTG的浓度范围为1至1000μg/L，LLOQ为1μg/L。该测定方法的准确度在90.5%至108.1%之间。六种分析物的提取回收率和基质效应分别在72.2%至95.5%和79.2%至98.4%之间。根据稳定性试验，大鼠血浆中的六种分析物在分析过程中是稳定的。在该测定方法验证的基础上，对大鼠口服藜芦提取物后六种甾体生物碱的药代动力学进行了研究。
