Hu Fengli, Deng Chunhui, Liu Yang, Zhang Xiangmin
Department of Chemistry, Fudan University, Shanghai 200433, China.
Talanta. 2009 Feb 15;77(4):1299-303. doi: 10.1016/j.talanta.2008.09.003. Epub 2008 Sep 11.
The chlorogenic acid (CA) in Honeysuckle is determined and identified by nano-liquid chromatography-electrospray ionization mass spectrometry (nano-LC-ESI/MS) after extraction with microwave-assisted extraction (MAE). As a new sample preparation method for Honeysuckle, the MAE procedure is optimized, validated and compared with conventional methods including reflux extraction (RE) and ultrasonic extraction (USE). It is found that MAE gives the best result due to the highest extraction efficiency within shortest extraction time (only 4 min). Here, CA is determined by nano-LC-ESI/MS based on the calibration curve of its authentic standard. The method linearity, detection limit, precision and recovery are studied. The results show that the combined MAE and nano-LC-ESI/MS method has a linearity (R(2) 0.991, 0.8-20 ng mL(-1)), a low limit of detection (0.5 ng mL(-1)), good precision (R.S.D.=2.54%) and a recovery (84.8%). The experiment has demonstrated that the nano-LC-ESI/MS following MAE is a fast and reliable method for quantitative analysis of CA in Honeysuckle.
采用微波辅助萃取（MAE）法提取金银花中的绿原酸（CA），然后用纳米液相色谱-电喷雾电离质谱（nano-LC-ESI/MS）对其进行测定和鉴定。作为一种用于金银花的新型样品制备方法，对MAE程序进行了优化、验证，并与包括回流萃取（RE）和超声萃取（USE）在内的传统方法进行了比较。结果发现，MAE由于在最短的萃取时间（仅4分钟）内具有最高的萃取效率，因而得到了最佳结果。在此，基于CA标准品的校准曲线，采用nano-LC-ESI/MS对其进行测定。研究了该方法的线性、检测限、精密度和回收率。结果表明，MAE与nano-LC-ESI/MS联用方法具有线性关系（R(2)=0.991，0.8 - 20 ng mL(-1)）、低检测限（0.5 ng mL(-1)）、良好的精密度（R.S.D.=2.54%）和回收率（84.8%）。实验表明，MAE后的nano-LC-ESI/MS是一种快速、可靠的金银花中CA定量分析方法。
