School of Traditional Chinese Medicine, Capital Medical University, 10 Youanmen, Xitoutiao, Beijing 100069, China.
School of Traditional Chinese Medicine, Capital Medical University, 10 Youanmen, Xitoutiao, Beijing 100069, China.
Food Chem. 2015 Jun 15;177:191-6. doi: 10.1016/j.foodchem.2015.01.033. Epub 2015 Jan 9.
A simple, effective and suitable UFLC-ESI-MS/MS method was firstly developed to simultaneously determine five characteristic constituents (piperine, piperlonguminine, Δα,β-dihydropiperlonguminine, pellitorine and piperanine) of Piper longum L. The total alkaloids of P. longum L. was prepared. The alkaloid contents of Piper nigrum L. and P. longum L. were compared. The analysis was carried out in multiple reaction monitoring scan mode. The method showed a good specificity, linearity (R(2)>0.995), stability (RSD<2.53%), repeatability (RSD<2.58%), and recovery (90.0-103.5%). The limits of detection and limits of quantification of five alkaloids were in the range of 0.02-0.03 and 0.05-0.10 ng/mL, respectively. The intra- and inter-day precision was less than 9.30% and 9.55%, respectively. The validation results confirmed that the method could simultaneously determine the target alkaloids in the sample. Furthermore, the identities of the alkaloids were verified by HPLC-ESI-MS/MS. Compared with P. nigrum, P. longum had lower piperine content but was enriched in the other four alkaloids.
首次建立了一种简单、有效、适用的 UFLC-ESI-MS/MS 方法，用于同时测定胡椒（Piper longum L.）中五种特征成分（胡椒碱、荜茇明碱、Δα,β-二氢胡椒明碱、白胡椒碱和胡椒堿）。制备了胡椒总生物碱。比较了黑胡椒（Piper nigrum L.）和荜茇（P. longum L.）中的总生物碱含量。采用多反应监测扫描模式进行分析。该方法具有良好的特异性、线性（R(2)>0.995）、稳定性（RSD<2.53%）、重复性（RSD<2.58%）和回收率（90.0-103.5%）。五种生物碱的检测限和定量限分别在 0.02-0.03 和 0.05-0.10 ng/mL 范围内。日内和日间精密度均小于 9.30%和 9.55%。验证结果证实，该方法可同时测定样品中的目标生物碱。此外，通过 HPLC-ESI-MS/MS 验证了生物碱的身份。与黑胡椒相比，荜茇中胡椒碱的含量较低，但其他四种生物碱的含量丰富。
