顶空固相微萃取-气相色谱-质谱法用于白术中挥发性成分的分析

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

采用顶空固相微萃取-气相色谱-质谱法(H S-SPME-GC-M S)分离鉴定了白术中的挥发性成分,并与采用传统的水蒸气蒸馏法(SD)提取的挥发性成分进行了比较。实验中筛选了固相微萃取纤维头,优化了SPME的操作条件。样品在70℃下平衡30m in后,用65μm聚二甲基硅氧烷-二乙烯基苯(PDM S-DVB)纤维头对白术样品顶空吸附30m in,于250℃下解吸4m in,然后采用GC-M S对解吸物进行分离鉴定;采用H S-SPME-GC-M S鉴定出41种组分,占总峰面积的90.81%;采用SD-GC-M S鉴定出31个组分,占总峰面积的88.19%,且采用SD所提取的组分基本上都被固相微萃取所提取。结果表明,H S-SPME可取代耗时的SD用于白术中挥发性物质的提取。

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 （SD-GC-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 [ 6.3.0.1 （ 2,3 ） ] 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 trans-β-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.