Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Ministry of Education, Wuhan University School of Pharmaceutical Sciences, Wuhan, China.
State Key Laboratory of Transducer Technology, Chinese Academy of Sciences, Beijing, China.
J Sep Sci. 2017 Dec;40(23):4628-4635. doi: 10.1002/jssc.201700815. Epub 2017 Oct 30.
Nonaqueous capillary electrophoresis with mass spectrometry has advantages for the analysis of active components in herbs. Here, a rapid nonaqueous capillary electrophoresis with mass spectrometry method was developed to separate, identify, and quantify palmatin, columbin, cepharanthine, menisperine, magnoflorine, and 20-hydroxyecdysone in Radix tinosporae. Electrospray ionization MS spectra of the six components were collected and possible cleavage pathways of main fragment ions were elucidated. The conditions that could affect separation, such as the composition of running buffer and applied voltage, were studied, and the conditions that could affect the mass spectrometry detection, such as the composition and flow rate of sheath liquid, the pressure of nitrogen gas, and the temperature and flow rate of the dry gas, were also optimized. Under the optimized conditions, the correlation coefficient was >0.99. The relative standard deviations of migration time and peak areas were <10%. The recoveries were calculated to be 99.31-107.80% in real samples. It has been demonstrated that the proposed method has good potential to be applied to determine the six bioactive components in Radix tinosporae.
非水毛细管电泳-质谱联用技术在中草药活性成分分析方面具有优势。本研究建立了一种快速非水毛细管电泳-质谱法，用于分离、鉴定和定量土槿皮乙酸、长春胺、蝙蝠葛碱、防己诺林碱、厚朴酚、20-羟基蜕皮甾酮在桃儿七中的含量。采集了这 6 个成分的电喷雾电离质谱谱图，并对主要碎片离子的可能裂解途径进行了阐述。研究了影响分离的条件，如运行缓冲液的组成和施加电压，以及影响质谱检测的条件，如鞘液的组成和流速、氮气压力、干燥气体的温度和流速等，优化了这些条件。在优化条件下，相关系数>0.99。迁移时间和峰面积的相对标准偏差<10%。在实际样品中，回收率计算为 99.31%-107.80%。研究表明，该方法具有良好的潜力，可用于测定土槿皮乙酸中这 6 种生物活性成分。
