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Abstract: A headspace solid-phase microextraction (HS-SPME) method followed by gas chromatography–mass spectrometry (GC–MS) is described for the analysis of volatile compounds in the dry rhizome of Ligusticum chuanxiong Hort. Three types of SPME fibers including PDMS, PDMS–DVB and DVB–CAR–PDMS were investigated and the best extraction was achieved with the mixed fiber DVB–CAR–PDMS. Parameters for HS-SPME in terms of temperature and time, sample amount and particle size, and desorption time were also investigated. A polar capillary column was used for the chromatographic separation. As a result, 73 compounds were determined and identified by the HS-SPME–GC–MS method with at least 20 more compounds than those in the methods available. Comparison was made between HS-SPME–GC–MS and steam distillation (SD)-GC–MS methods. Using much less sample amount, shorter extraction time and simpler procedure, HS-SPME method can achieve similar results with those by SD. In conclusion, the present method is simple, rapid and effective and can be used for the analysis of volatile compounds in medicinal plants. [Copyright &y& Elsevier]

Abstract: A novel and rapid headspace solvent microextraction followed by gas chromatography–mass spectrometry (HSME-GC–MS) for the analysis of the volatile compounds of Foeniculum vulgare Mill is described. HSME parameters including extracting solvent, extraction temperature and time, headspace volume and particle size were optimized. As a result, benzyl alcohol was finally used for the extraction at 70°C for 20min with headspace volume of 12.1ml and particle size of 120 mesh. Under the determined conditions, the powered samples of Foeniculum vulgare Mill were directly applied for the analysis. A comparison of HSME-GC–MS, solid phase microextraction (SPME)-GC–MS and steam distillation (SD)-GC–MS methods was made and showed that the HSME-GC–MS method was simple, inexpensive and effective and can be used for the analysis of volatile compounds in traditional Chinese medicines (TCMs). [Copyright &y& Elsevier]