Deng Chunhui, Ji Jie, Li Ning, Yu Yingjia, Duan Gengli, Zhang Xiangmin
Department of Chemistry, Fudan University, Shanghai 200433, China.
J Chromatogr A. 2006 Jun 9;1117(2):115-20. doi: 10.1016/j.chroma.2006.03.066. Epub 2006 May 5.
Curcumol, germacrone and curdione are the main active ingredients in a common traditional Chinese medicine (TCM) of Rhizoma Curcuma, and commonly used as the TCM quality control markers. In the present work, microwave-assisted extraction (MAE) followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was developed for the quantitative analysis of curcumol, curdione and germacrone in Rhizoma Curcuma. The MAE and HS-SPME parameters were studied, and the method was validated. The optimal MAE conditions obtained were: microwave power of 700 W and irradiation time of 4 min, and HS-SPME optimal conditions were: fiber coating of 100 microm PDMS, extraction temperature of 80 degrees C, extraction time of 20 min, stirring rate of 1,100 rpm, and salt concentration of 30% NaCl. The proposed method provided good precision (RSD less than 12%) and recoveries between 86% and 93%. The proposed method was applied to the determination of the three marker compounds in three species of Curcuma rhizomes (Curcuma wenyujin, Curcuma phaeocaulis, and Curcuma kwangsiensis). To demonstrate the proposed method reliability, a conventional technique of steam distillation was also used for the analysis of curcumol, germacrone and curdione in the TCMs. The results show that MAE-HS-SPME is a simple, rapid, solvent-free and reliable method for the determination of curdione, curcumol and germacrone in TCM, and also a potential and powerful tool for quality assessment of Rhizoma Curcuma.
莪术醇、吉马酮和莪术二酮是常用中药莪术的主要活性成分,常被用作中药质量控制指标。在本研究中,建立了微波辅助萃取(MAE)结合顶空固相微萃取(HS-SPME)和气相色谱-质谱联用(GC-MS)的方法,用于莪术中莪术醇、莪术二酮和吉马酮的定量分析。研究了MAE和HS-SPME的参数,并对该方法进行了验证。获得的最佳MAE条件为:微波功率700 W,辐照时间4 min;HS-SPME的最佳条件为:100 μm PDMS纤维涂层,萃取温度80℃,萃取时间20 min,搅拌速率1100 rpm,盐浓度30% NaCl。该方法具有良好的精密度(RSD小于12%),回收率在86%至93%之间。该方法应用于三种莪术根茎(温郁金、蓬莪术和广西莪术)中三种指标化合物的测定。为证明该方法的可靠性,还采用传统的水蒸气蒸馏技术对中药中的莪术醇、吉马酮和莪术二酮进行了分析。结果表明,MAE-HS-SPME是一种简单、快速、无溶剂且可靠的测定中药中莪术二酮、莪术醇和吉马酮的方法,也是莪术质量评价的一种潜在且有力的工具。