[关键词]
[摘要]
目的 应用超高效液相色谱串联四级杆飞行时间质谱(UPLC-Q-TOF-MS/MS)定性分析多物料多流程炮制半夏Pinellia ternata的化学成分,分阶段探究不同物料和流程对其成分的影响。比较成分差异性,为阐明多物料多流程炮制对化学成分的变化规律提供参考。方法 将通过不同物料和炮制流程得到的半夏阶段产物分为4组,分别为浸漂半夏、石灰制半夏、甘草制半夏、法半夏,以生半夏作为对照。以5种样品醇提液为供试品溶液,采用Waters Acquity BEH C18色谱柱,乙腈-0.1%甲酸水为流动相进行二元梯度洗脱,质谱采用电喷雾离子化源(ESI),正、负离子全扫描的一级和二级质谱信息。结果 通过一级精确质荷比和二级的碎片数据,参考文献、数据库以及质谱裂解规律,对5组样品所含成分进行鉴定。鉴定了101个化学成分,分别为7个生物碱类、5个氨基酸类、5个酰胺类、14个醇胺类、26个黄酮类、6个溶血磷脂酰胆碱类、14个脂肪酸甘油脂类、6个有机酸类、7个皂苷类及11个其他类型化合物。结论 通过UPLC-Q-TOF-MS/MS对5组样品化学成分进行分析,发现半夏炮制前后化学成分存在明显差异,物料甘草为半夏引入了甘草黄酮、三萜皂苷类成分,而物料石灰对成分引入影响不大,推测出石灰的加入是为了在不影响药效成分的前提下减轻半夏毒性。与生品相比,浸漂后的半夏成分减少,推测浸漂的过程中,会使成分有所损失。而经过多物料多流程炮制的法半夏减少了刺激性毒性成分,增加了甘草黄酮类成分。该方法快速、准确,为探究半夏多物料多流程炮制机制提供一种新的策略,对其药效物质深入研究及质量控制具有重要意义。
[Key word]
[Abstract]
Objective To analyze the chemical constituents of Banxia (Pinellia ternata) processed by multi-material and multi-process by ultra-high performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS/MS), and explore the effects of different materials and processes on its constituents. Through comparing the difference of components, to provide reference for elucidating the change rule of chemical components of P. ternata before and after processing. Methods The varieties of P. ternata obtained by different materials and processing procedures were divided into four groups:soaked P. ternata, P. ternata made of lime, P. ternata made of Glycyrrhizae Radix et Rhizoma and Fabanxia (Pinelliae Rhizoma Praeparatum). P. ternata was used as a control. The alcohol extracts of five samples were used as the donor solution, Waters Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used, acetonitrile-0.1% formic acid water was used as the mobile phase for binary gradient elution, electrospray ionization source (ESI) was used for mass spectrometry, and the primary and secondary mass spectra information of positive and negative ion full scan was used. Results The components contained in the five groups of samples were identified by the first order exact mass to charge ratio, the second level fragment data, references or databases, and the law of mass spectrometry fragmentation. A total of 101 chemical constituents were preliminarily characterized, including seven alkaloids, five amino acids, five amides, 14 alcoholamines, 26 flavonoids, six lysophosphatidylcholines, 14 fatty acid glycerolipids, six organic acids, seven saponins, and 11 compounds of other types. Conclusion UPLC-Q-TOF-MS/MS is used to analyze the chemical constituents of different processed varieties of P. ternata, and it is found that there are significant differences in the chemical constituents before and after processing of P. ternata. Glycyrrhiza uralensis introduces licoflavone and triterpene saponins for P. ternata, while lime has little effect on the introduction of components. It is speculated that the addition of lime is to reduce the toxicity of P. ternata without affecting the pharmacodynamic components. Compared with raw products, the components of P. ternata decreased after soaking, and it was speculated that the components of P. ternata may be lost during soaking. P. ternata, which is processed through multiple materials and multiple processes, reduces the irritating and toxic ingredients and increases the licoflavone. This method is rapid and accurate, providing a new strategy for exploring the multi-process processing mechanism of P. ternata, which is of great significance for the in-depth study of its pharmacodynamic substances and quality control.
[中图分类号]
R284.1;R283.6
[基金项目]
国家重点研发计划(2018YFC1707201)