顶空固相微萃取气相色谱质谱联用法分析马油挥发物组成及其腥味物质

Analysis of volatile compounds and the smell substance in horse oil by head space solid-phase micro-extractions gas chromatography-mass spectrometry

中文关键词:  马油  挥发性成分  顶空固相微萃取  气相色谱质谱联用法

英文关键词:horse oil  volatile components  head space solid-phase micro-extractions  gas chromatography-mass spectrometry

中文摘要:

      目的 建立顶空固相微萃取气相色谱质谱联用法分析马油挥发物组成, 并初步判断马油主要腥味物质。方法 采用顶空固相微萃取(head space solid-phase micro-extractions, HS-SPME)、气相色谱-质谱(gas chromatography-mass spectrometry, GC-MS)联用技术, 通过单因素与响应面分析, 以分离的峰个数和峰面积为考察指标, 建立马油挥发性物质的分析方法。根据马脂肪、炼制马油、粗马油和精制马油这4种样品的挥发性成分物质种类的变化, 可初步判断马油腥味成分的种类。结果 HS-SPME最佳条件为65 μm聚二乙烯苯/聚二甲基硅氧烷(divinylbenzene/polydimethylsiloxane, DVB/PDMS)微萃取头、萃取温度83 ℃、平衡时间40 min、萃取时间59 min、样品用量4.500 g、解吸时间5 min。确定了43种化合物结构, 初步判断己醛、Z-2-庚烯醛、反-2-辛烯醛、壬醛、反-2-壬烯醛、癸醛、反, 反-2, 4-壬二烯醛、反-2-癸烯醛、反, 反-2, 4-癸二烯醛、2-十一烯醛为马油腥味成分。结论 该方法可用于马油挥发性成分的分析, 并初步判断马油腥味成分的种类。

英文摘要:

      Objective To establish an analytical method for the volatile composition of horse oil by head space solid-phase micro-extractions gas chromatography-mass spectrometry (HS-SPME-GC-MS), and judge the main smell material of horse oil. Methods The volatile compounds in horse oil were analyzed by HS-SPME-GC-MS, combined with single-factor and response-surface, and the peak number and peak area were used as indexes to establish an optimal method for the analysis of volatile substances in horse oil. According to the changes of the types of volatile components and the threshold value of volatile substances in 4 kinds of samples, such as horse fat, refined horse oil, crude horse oil and purified horse oil, the types of odorization ingredients of horse oil could be preliminarily judged. Results The optimal extraction parameters were achieved on HP-5MS column under the following conditions: 65 μm divinylbenzene/polydimethylsiloxane (DVB/PDMS) solid-phase micro extraction fiber, extraction 4.500 g of sample for 59 min at 83 ℃, 40 min equilibration and 5 min desorption. Forty-three kinds of compound structure were determined, which was preliminarily judged that the smell of horse oil was mainly caused by hexanal, Z-2-heptenal, (E)-2-octenal, nonanal, (E)-2-nonenal, decanal, (E,E)-2,4-nonadienal, (E)-2-decenal, (E,E)-2,4-dodecadienal, 2-undecenal. Conclusion This method can be used for the analysis of volatile components of horse oil, and can determine the type of the smell of horse oil.