Wei Jinxia, Jiang Zhen, Cui Zhi, Guo Xingjie
Department of Analytical Chemistry, School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang, 110016, Liaoning, China.
Anal Bioanal Chem. 2015 Jul;407(18):5535-40. doi: 10.1007/s00216-015-8704-4. Epub 2015 May 7.
The objective of this study was to develop a rapid and reliable homogenate extraction (HGE) and ultra high-performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method for simultaneous analysis of eight bioactive oxoisoaporphine alkaloids (including two new alkaloids) in Rhizoma Menispermi. HGE was optimized by response surface methodology (RSM) to obtain the maximum extraction efficiency of eight alkaloids. Separation was achieved on a Waters ACQUITY UPLC® BEH C18 column (50 × 2.1 mm(2), 1.7 μm) using gradient elution with a mobile phase consisting of acetonitrile and 0.2% formic acid in water. Quantification was performed with multiple reaction monitoring (MRM) mode using positive ESI as an interface. This is the first report of the simultaneous analysis of eight oxoisoaporphine alkaloids in Rhizoma Menispermi using a UPLC-MS/MS method; this analysis afforded good linearity, precision, and accuracy. Then, the method was successfully applied to determine the alkaloids in Rhizoma Menispermi from different sources.
本研究的目的是开发一种快速可靠的匀浆提取(HGE)和超高效液相色谱 - 串联质谱(UPLC-MS/MS)方法,用于同时分析北豆根中8种具有生物活性的氧化异阿朴啡生物碱(包括2种新生物碱)。采用响应面法(RSM)对HGE进行优化,以获得8种生物碱的最大提取效率。在Waters ACQUITY UPLC® BEH C18柱(50×2.1 mm²,1.7μm)上进行分离,使用由乙腈和0.2%甲酸水溶液组成的流动相进行梯度洗脱。采用正离子电喷雾电离(ESI)作为接口,在多反应监测(MRM)模式下进行定量分析。这是首次报道采用UPLC-MS/MS方法同时分析北豆根中8种氧化异阿朴啡生物碱;该分析具有良好的线性、精密度和准确度。然后,该方法成功应用于测定不同来源北豆根中的生物碱。