[关键词]
[摘要]
目的 应用固相萃取结合超高效液相色谱-电喷雾四级杆飞行时间质谱联用技术(UPLC-Q-TOF-MS),对黄精九蒸九晒炮制过程中的化学成分进行分析鉴定。方法 采用ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7 μm),以乙腈-0.1%甲酸水作为流动相梯度洗脱,体积流量0.3 mL/min,在电喷雾负离子模式下进行检测,四级杆飞行时间串联质谱对各主要色谱峰进行归属。结果 根据所获得的精确相对分子质量,同时结合色谱保留行为、质谱裂解规律、特征碎片离子、对照品比对以及相关文献报道,共鉴定炮制前后黄精中的61个化学成分,包括16个甾体皂苷类成分、12个黄酮类成分、5个木脂素类成分、1个香豆素类成分、3个生物碱类成分、4个脂肪酸类成分、3个氨基酸类成分、2个糖类成分、4个酯类成分、1个醛类成分、1个有机酸类成分及9个未知成分。结论 炮制对黄精中的化学成分影响很大,随着炮制时间的增加如成分异构化、原生苷种类以及含量减少、苷元含量的增加等。九蒸九晒黄精增效作用炮制或许与其化学成分变化有关,为黄精九蒸九晒炮制机制的研究提供理论依据,为黄精的进一步开发利用提供科学依据。
[Key word]
[Abstract]
Objective To analyze and identify the chemical constituents in the processing of Huangjing (Polygonati Rhizoma) after "nine times steaming and nine times sunning" by solid-phase extraction combined with ultra performance liquid chromatography electrospray ionization time of flight mass spectrometry (UPLC-Q-TOF-MS).Methods ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) was used as gradient elution with acetonitrile-0.1% formic acid as mobile phase. Volume flow 0.3 mL/min was detected under electrospray ionization mode. The main chromatographic peaks were assigned by four stage time of flight mass spectrometry. Results According to the obtained accurate molecular weight, combined with the chromatographic retention behavior, mass spectrometry cleavage, characteristic fragment ions, reference comparison, and relevant literature reports, a total of 61 chemical components were identified in aqueous extracts and fermentation both from Polygonati Rhizoma, including 16 steroidal saponins, 12 flavonoid components, five lignin components, one coumarin components, three alkaloid components, four fatty acid components, three amino acid components, two carbohydrate components, four ester components, one aldehyde components, one organic acid component and nine unknown ingredients.Conclusion Processing has a great influence on the chemical components of Polygonati Rhizoma, with the increase of processing time, such as component isomerization, the type and content of primary glycosides decrease, and the content of aglycones increase.The enhancing effect of nine times processing of Polygonati Rhizoma may be related to the change of chemical composition. This study can provide theoretical basis for the study of the processing mechanism of Polygonati Rhizoma, and provide scientific basis for the further development and utilization of Polygonati Rhizoma.
[中图分类号]
R284.1
[基金项目]