Chen Junhui, Wang Fengmei, Liu Jie, Lee Frank Sen-Chun, Wang Xiaoru, Yang Huanghao
QingDao Key Lab on Analytical Technology Development and Standardization of Chinese Medicines, First Institute Oceanography of SOA, Qingdao 266061, China.
Anal Chim Acta. 2008 Apr 21;613(2):184-95. doi: 10.1016/j.aca.2008.02.060. Epub 2008 Mar 5.
A new method based on accelerated solvent extraction (ASE) followed by ultra performance liquid chromatography (UPLC) analysis has been developed for the identification and quantification of major alkaloids in extracts of Coptis chinensis Franch. The UPLC system consisted of a dual detection system of photodiode array detector (PDA) and positive ion electrospray ionization-tandem mass spectrometry (ESI-MS/MS) in sequential configuration. The operational parameters of ASE including extraction solvent, extraction temperature, static extraction time and extraction cycles were optimized. UPLC analysis was performed on an ACQUITY UPLC BEH C(18) column eluted by a mobile phase of acetonitrile spiked with a buffer solution consisting of 0.50% acetic acid and 20 mmol L(-1) ammonium acetate. A tandem quadrupole spectrometer operating in either full scan mode or in MS/MS mode for multiple reaction monitoring (MRM) was used for the identification and quantitative analysis of eight major alkaloids in C. chinensis Franch extracts. The samples were also analyzed on a high-performance liquid chromatography-electrospray ionization-time-of-flight mass spectrometry (HPLC-ESI-TOF-MS) system to confirm the identification results. Three of the eight major alkaloids, berberine, palmatine and jatrorrhizine were quantified by UPLC-PDA and UPLC-MS/MS. The results indicated that both UPLC-PDA and UPLC-MS/MS methods were simple, sensitive and reliable for the determination of alkaloids in C. chinensis Franch. Seven Huanglian samples from different locations were analyzed using the established methods. UPLC fingerprints based on the distribution of the eight major alkaloids can serve as a rapid and reliable method for the authentication and quality evaluation of traditional Chinese medicine (TCM) herbs.
建立了一种基于加速溶剂萃取(ASE)结合超高效液相色谱(UPLC)分析的新方法,用于黄连提取物中主要生物碱的鉴定和定量分析。UPLC系统由光电二极管阵列检测器(PDA)和正离子电喷雾电离串联质谱(ESI-MS/MS)的双检测系统组成,呈串联配置。对ASE的操作参数,包括萃取溶剂、萃取温度、静态萃取时间和萃取次数进行了优化。UPLC分析在ACQUITY UPLC BEH C18柱上进行,流动相为乙腈,加入由0.50%乙酸和20 mmol L-1乙酸铵组成的缓冲溶液。使用串联四极杆光谱仪在全扫描模式或多反应监测(MRM)的MS/MS模式下对黄连提取物中的8种主要生物碱进行鉴定和定量分析。还在高效液相色谱-电喷雾电离飞行时间质谱(HPLC-ESI-TOF-MS)系统上对样品进行分析,以确认鉴定结果。通过UPLC-PDA和UPLC-MS/MS对8种主要生物碱中的3种,即小檗碱、巴马汀和药根碱进行了定量分析。结果表明,UPLC-PDA和UPLC-MS/MS方法对于黄连中生物碱的测定均简便、灵敏且可靠。使用所建立的方法对7个来自不同产地的黄连样品进行了分析。基于8种主要生物碱分布的UPLC指纹图谱可作为一种快速可靠的方法用于中药药材的鉴定和质量评价。