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Headspace Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry for Analysis of Volatile Components from Atractlodes macrocephala Koidz.

GUO Fangqiu~1,HUANG Lanfang~(1,2),ZHOU Shaoyun~1 (1.Research Center for Modernization of Chinese Herbal Medicine,College of Chemistry and Chemical Engineering,Central South University,Changsha 410083,China;2.Technical Center of Changde Cigarette Factory,Changde 415000,China)  
Headspace solid-phase microextraction(HS-SPME) technique was employed to extract the volatile components from Chinese traditional medicine,Atractlodes macrocephala Koidz.The volatile components were isolated and identified successfully by gas chromatography-mass spectrometry(GC-MS).The results from HS-SPME-GC-MS were compared with those obtained from steam distillation-GC-MS(SDGC-MS) with a good agreement.The volatiles were collected using a polydimethylsiloxane-divinylbenzene(PDMS-DVB) fiber by HS-SPME.The best response was obtained when the extraction temperature was 70 ℃,the equilibrium time and extraction time were all 30 min and the desorption time was 4 min.Analysis was performed by GC-MS with a polysiloxane capillary column(30 m×0.25 mm,film thickness 0.25 μm) using He as the carrier gas and a programmed temperature run.Forty-one components accounting for 90.81% were(identified).The main components(relative amount more than 1%) of the samples by HS-SPME were atractylone(40.12%),γ-elemene(14.73%),aromadendrene(13.05%),eudesma-4(14),11-diene(5.46%),caryophyllene(2.56%),patchoulene(2.55%),6,10,11,11-tetramethyl-tricyclo[,3)]undec-7-ene(2.11%),cedrene(1.48%),α-caryophyllene(1.48%) and selina-4(14)-7(11)diene-8-one(1.01%).By SD-GC-MS,31 components accounting for 88.19% were identified and all these components could be extracted by SPME except transβ-ocimene which accounts only 0.10%.The results showed that the HS-SPME technique can be used to extract the the volatile components from Atractlodes macrocephala Koidz.in place of the traditional time-consuming SD.
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