微波精馏-固相微萃取-气相色谱-质谱联用快速测定红花中挥发性成分

Yingjia Yu, Bei Yang, Tao Zhou, Haiying Zhang, Luping Shao, Gengli Duan
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引用次数: 6

摘要

本文建立了微波精馏-固相微萃取-气相色谱-质谱联用技术(MD-SPME/GC-MS)分析红花中主要成分的方法。采用MD-SPME技术,红花中挥发物的分离、提取和浓缩仅需一步完成。对SPME纤维涂层、微波功率、辐照时间、加水量等影响提取效率的参数进行了优化。得到的最佳实验参数为:65 μm CW/DVB SPME纤维,微波功率400 W,辐照时间3 min,水体积1 mL。并将该方法与常规蒸汽蒸馏法(SD)进行了比较。采用MD-SPME - GC-MS分离鉴定了红花中32个化合物,主要有丹皮酚、α -细辛酮、β -细辛酮、1-甲基-4-(2-丙烯基)苯和二乙基苯,而常规SD - GC-MS只分离鉴定了18个化合物。相对标准偏差(rsd)值小于10%,表明该方法重现性好。结果表明,MD-SPME/GC-MS是一种简便、快速、有效的红花挥发油成分分析方法。
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Rapid Determination of Volatile Constituents in Safflower by Microwave Distillation and Simultaneous Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

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 μm 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.

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