Yu Yingjia, Yang Bei, Zhou Tao, Zhang Haiying, Shao Luping, Duan Gengli
Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, Shanghai 200032, PR China.
Ann Chim. 2007 Oct;97(10):1075-84. doi: 10.1002/adic.200790091.
In this paper, microwave distillation and solid-phase microextraction coupled with gas chromatography-mass spectrometry (MD-SPME/GC-MS) was developed for the analysis of essential components in safflower. Using the MD-SPME technique, the isolation, extraction and concentration of volatile compounds in safflower were carried out in only one step. Some parameters affecting the extraction efficiency such as SPME fiber coating, microwave power, irradiation time and the volume of water added were optimized. The optimal experiment parameters obtained were: 65 microm CW/DVB SPME fiber, a microwave power of 400 W, an irradiation time of 3 min and water volume of 1 mL. The proposed method has been compared with conventional steam distillation (SD) for extraction of essential oil compounds in safflower. Using MD-SPME followed by GC-MS, 32 compounds in safflower were separated and identified, which mainly included paeonol, alpha-asarone, beta-asarone, 1-methyl-4-(2-propenyl)-benzene and diethenyl-benzene, whereas only 18 compounds were separated and identified by conventional SD followed by GC-MS. The relative standard deviation (R.S.D.) values of less than 10% show that the proposed method has good reproducibility. The results show that MD-SPME/GC-MS is a simple, rapid, effective method for the analysis of volatile oil components in safflower.
本文建立了微波蒸馏-固相微萃取联用气相色谱-质谱法(MD-SPME/GC-MS)用于分析红花中的主要成分。采用MD-SPME技术,仅一步即可实现红花中挥发性化合物的分离、萃取和浓缩。对影响萃取效率的一些参数,如SPME纤维涂层、微波功率、辐照时间和加水量进行了优化。得到的最佳实验参数为:65μm CW/DVB SPME纤维、400W微波功率、3min辐照时间和1mL水量。将该方法与传统水蒸气蒸馏(SD)法用于红花中精油化合物的萃取进行了比较。采用MD-SPME结合GC-MS,分离鉴定出红花中的32种化合物,主要包括丹皮酚、α-细辛脑、β-细辛脑、1-甲基-4-(2-丙烯基)-苯和二乙烯基苯,而传统SD结合GC-MS仅分离鉴定出18种化合物。相对标准偏差(R.S.D.)值小于10%表明该方法具有良好的重现性。结果表明,MD-SPME/GC-MS是一种分析红花挥发油成分的简单、快速、有效的方法。