顶空固相微萃取-气相色谱-质谱联用法分析椪柑芳香水中挥发性成分

Headspace Solid-phase Microextraction-Gas Chromatography-Mass Spectrometry for Analysis of Key Volatile Compounds in Aromatic Water from Ponkan

采用顶空固相微萃取-气相色谱-质谱联用法（HS-SPME-GC/MS）分离鉴定椪柑芳香水中的挥发性成分,研究固相微萃取头种类（PDMS/DVB 65μm,CAR/PDMS 75μm和DVB/CAR/PDMS 50/30μm）、吸附温度（30-50℃）、吸附时间（5-30 min）和样品体积（2-10 mL）对椪柑芳香水分离效果的影响。试验结果表明,采用DVB/CAR/PDMS固相微萃取头,样品体积8 mL,在温度40℃下吸附20 min,能达到最佳吸附效果。椪柑芳香水中主要的挥发性成分为：d-柠檬烯40.85%,乙醇17.17%,α-萜品醇15.61%,1-辛醇6.20%,β-月桂烯3.48%,3-甲基-1-丁醇3.01%,β-芳樟醇2.93%,樟脑2.88%,辛酸乙酯2.34%,α-蒎烯1.47%,占峰面积总和的95.94%。对顶空固相微萃取法进行重复性试验,10种挥发性成分的相对标准偏差（RSD）均低于7.0%,表明应用HS-SPMEGC/MS联用技术可对椪柑芳香水中挥发性成分进行快速、准确地分析。

For the fist time, key volatile compounds in the headspace of aromatic water from ponkan has been analyzed using headspace solid-phase microextraction（HS-SPME） combined with gas chromatography-mass spectrometry（GC-MS）. The effects of SPME fiber（PDMS/DVB 65 μm, CAR/PDMS 75 μm and DVB/CAR/PDMS 50/30 μm）, adsorption temperature（30-50 ℃）, adsorption time（5-30 min） and sample volume（2-10 mL） were studied to developHSSPME condition for obtaining the highest extraction efficiency. For the headspace volatile extraction, the optimum conditions were： DVB/CAR/PDMS fiber, 8 ml of sample volume, adsorption at 40 ℃ for 20 min. The main volatile flavor compounds were： d-limonene, 40.85%; ethanol, 17.17%; α-terpineol, 15.61%; 1-octanol, 6.20%; β-myrcene, 3.48%;3-methyl-1-butanol, 3.01%; β-linalool, 2.93%; naphthalene, 2.88%; ethyl caprylate, 2.34%; α-pinene, 1.47%. Ten kinds of compounds accounted for 95.94% of total peak area. Relative standard deviation（RSD） for three replicate analyses was found to be less than 7.0% and confirmed the feasibility of the HS-SPME-GC/MS technique for headspace analysis of key volatile compounds in aromatic water from ponkan.