Fu Xiaohong, Chen Hua, Yang Fengqing, Xia Zhining
College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044, China.
Se Pu. 2012 May;30(5):515-21. doi: 10.3724/sp.j.1123.2011.11024.
A novel method of microwave assisted solid phase headspace gas chromatography (MASP-HSGC) was developed through online coupling of solvent-free microwave extraction (SFME) and headspace-gas chromatography via a six-way valve. The method can quickly and directly analyze the volatile compounds from solid samples with its ability of simultaneous extraction, separation and analysis without any pretreatment. The method was applied to analyze the volatile compounds of solid Curcuma. Some experimental parameters such as the chromatographic conditions, microwave power and irradiation time were studied. Curcumol was used as the standard to evaluate the recovery, the limit of detection and the contents of compounds in a Curcuma sample. The essential oils were prepared by hydrodistillation extraction (HD) and SFME separately, and analyzed by gas chromatography-mass spectrometry (GC-MS) to compare the results with those from the developed method. It showed that the numbers of compounds obtained by the three methods of HD-GC, SFME-GC and MASP-HSGC were 35, 33, 40 respectively. The contents of curcumol using the three methods were (0.294 +/- 0.015), (0.331 +/- 0.023), (0.297 +/- 0.009) mg/g respectively. The method was approved to be suitable for the rapid analysis of volatile components in Curcuma.
通过六通阀将无溶剂微波萃取（SFME）与顶空气相色谱在线联用，开发了一种新型的微波辅助固相顶空气相色谱法（MASP-HSGC）。该方法能够对固体样品中的挥发性化合物进行快速直接分析，具备同时萃取、分离和分析的能力，无需任何预处理。将该方法应用于分析固体姜黄中的挥发性化合物。研究了一些实验参数，如色谱条件、微波功率和辐照时间。以莪术醇为标准品，评估回收率、检测限以及姜黄样品中化合物的含量。分别采用水蒸馏萃取（HD）和SFME制备挥发油，并通过气相色谱-质谱联用（GC-MS）进行分析，将结果与所开发方法的结果进行比较。结果表明，HD-GC、SFME-GC和MASP-HSGC三种方法得到的化合物数量分别为35、33、40种。三种方法测得的莪术醇含量分别为（0.294±0.015）、（0.331±0.023）、（0.297±0.009）mg/g。该方法被证明适用于姜黄中挥发性成分的快速分析。
