热脱附-气相色谱/质谱联用分析初榨橄榄油挥发性风味成分
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摘要
以橄榄油为原料,分别采用液液萃取法、顶空法、固相微萃取法、热脱附法提取橄榄油风味成分,使用气相色谱-质谱法(GC-MS)结合Massworks~(TM)质谱解析软件鉴定分析,并针对最佳提取方法进行工艺优化。结果表明,热脱附法因操作简单、重复性好、无需溶剂及样品检测非破坏性等优点,适宜橄榄油风味成分的检出。最佳萃取条件为:吸附温度40℃;吸附时间2 h;一级解吸温度180℃;一级解吸时间5 min;二级解吸温度280℃;二级解吸时间8 min;冷阱温度-30℃。橄榄油风味成分共鉴定出26种,有醇类、醛类、酯类、酮类、烃类,不同国家的初榨橄榄油挥发性组分存在差异;同一国家的初榨橄榄油挥发性组分存在差异;同一国家不同等级橄榄油挥发性组分存在差异。
Taking olive oil as raw material, the flavor components of olive oil were extracted by liquid-liquid extraction, headspace method, solid-phase micro-extraction and thermal desorption, which was also determined and analyzed by gas chromatography-mass spectrometry( GC-MS) combined with Massworks~(TM) software,and optimize the process for the best extraction method. The results show that the thermal desorption method was suitable for the detection of olive oil flavor components due to its advantages of simple operation, good repeatability, no solvent and non-destructive testing of samples. The optimum extraction conditions were as follows : 40 ℃ adsorption temperature;2 h adsorption time; 180 ℃ primary desorption temperature; 5 min primary desorption time; 280 ℃ secondary desorption temperature; 8 min secondary desorption time;-30 ℃ cold trap temperature. A total of 26 olive oil flavor components were identified, including alcohols, aldehydes, esters, ketones, and hydrocarbons. There were differences in the volatile components of virgin olive oil in different countries; there were differences in the volatile components of virgin olive oil in the same country; differences in volatile components of Olive Oil of different grades in the same country.
Taking olive oil as raw material, the flavor components of olive oil were extracted by liquid-liquid extraction, headspace method, solid-phase micro-extraction and thermal desorption, which was also determined and analyzed by gas chromatography-mass spectrometry( GC-MS) combined with Massworks~(TM) software,and optimize the process for the best extraction method. The results show that the thermal desorption method was suitable for the detection of olive oil flavor components due to its advantages of simple operation, good repeatability, no solvent and non-destructive testing of samples. The optimum extraction conditions were as follows : 40 ℃ adsorption temperature;2 h adsorption time; 180 ℃ primary desorption temperature; 5 min primary desorption time; 280 ℃ secondary desorption temperature; 8 min secondary desorption time;-30 ℃ cold trap temperature. A total of 26 olive oil flavor components were identified, including alcohols, aldehydes, esters, ketones, and hydrocarbons. There were differences in the volatile components of virgin olive oil in different countries; there were differences in the volatile components of virgin olive oil in the same country; differences in volatile components of Olive Oil of different grades in the same country.
引文
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[14]杜学伟,王锴,杜光尧,等.热脱附/冷阱聚焦/气相色谱/质谱法卷烟香气分析[J].分析测试技术与仪器,2007,13(1):33-40DU Xuewei, WANG Kai, DU Guangyao, et al. Direct thermal desorption-cooled injection System-GC/MS analysis of flavor compounds in cigarette[J]. Analysis and Testing Technology and Instruments,2007,13(1):33-40
[15]高群英,高岩,张汝民,等.3种菊科植物香气成分的热脱附气质联用分析[J].浙江农林大学学报,2011,28(2):326-332GAO Qunying,GAO Yan,ZHANG Rumin, et al. Aromatic composition in three plant species using TDS-GC/MS[J].Journal of Zhejiang Forestry College,2011,28(2):326-332
[16]田怀香,王璋.热脱附-气质联用分析金华火腿挥发性风味[J].食品与机械,2007,23(3):10-13TIAN Huaixiang, WANG Zhang. Theuse of thermal desorption-GC-MS in volatile flavor profiling of jinhua ham[J].Food and Machinery, 2007,23(3):10-13
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[18] KALUA C M, ALLEN M S, BEDGOOD J. Olive oil volatile compounds, flavour development and quality:A critical review[J].Food Chemistry,2007,100:273-286
[19] VICHI S,PIZZALE L,CONTE L S. Solid-phase microextraction in the analysis of virgin olive oil volatile fraction:modification induced by oxidation and suitable markers of oxidative status[J]. Agricultural and Food Chemistry,2003,51:6564-6571
[20]向春蓉,徐洲,王寒冬,等.凉山州4个引进品种初榨橄榄油的品质分析[J].中国油脂,2017(3):144-147XIANG Chunrong, XU Zhou, WANG Handong, et al. Quality analysis of virgin olive oils from four introduced varieties in Liangshan[J]. China Oils and Fats, 2017(3):144-147
[21]PROCIDA G, GIOMO A, CICHELLI A,et al. Study of volatile compounds of detective virgin olive oils and sensory evaluation:Achemometric approach[J]. Science of Food and Agriculture, 2005,85:2175-2183
[22] MORALES M T, RIOS J J,APARICIA R. Changes in the volatile composition of virgin olive oil during oxidation:Flavors and off-flavors[J]. Agricultural and Food Chemistry,1997,45:2666-2673.
[2]庄小丽,相玉红,强洪,等.近红外光谱和化学计量学方法用于橄榄油品质分析与掺杂量检测[J].光谱学与光谱分析,2010,30(04):933-936ZHUANG Xiaoli, XIANG Yuhong, QIANG HONG, et al.Quality analysis of olive oil and quantification detection of adulteration in olive oil by Near-Infrared spectrometry and chemometrics[J]. Spectroscopy and Spectral Analysis,2010,30(04):933-936
[3]赵延胜,董英,王子君,等.近红外光谱和气相色谱-质谱联用技术对橄榄油掺杂及品质分析研究[J].现代科学仪器,2012,05:105-108ZHAO Yansheng, DONG Ying, WANG Zijun, et al. Adulteration and quality analysis of olive oil by Near-Infrared Spectrometry and gas chromatography-mass spectrometry[J].Modern Scientific Instruments, 2012,05:105-108
[4]杨柳,吴翠蓉,朱杰丽,等.顶空-气质联用法鉴别油茶籽油真伪[J].中国粮油学报,2012,11:105-113YANG Yichao, ZHANG Mingming, SUN Yuanmingl,et al.Contamination Status and Safety Evaluation of Phthalates in Edible Oil[J]. Journal of the Chinese Cereals and Oils Association, 2012,05:105-108
[5]刘平年.顶空气相色谱质谱联用法分析芝麻油的挥发性气味成分[J].中国油脂,2005,30(10):45-47LIU Pingnian. Volatile flavor components analysis of sesame seed oil by HS-GC-MS[J]. China Oils and Fats, 2005,30(10):45-47
[6]MITSUYA S, YUJI N, MASATOSI N. Headspace gas analysis of volatile compounds of light and deep roasted sesame seed oil[J].Food Sci Technol Int Tokyo, 1998,4(1):14-17
[7]HIROYUKI K, KOUICHI K, SHIGEO N. Relationship between the volatile components and the aromatic quality of roasted Sesame seed oils[J]. Journal of Oleo Science, 2002,51(11):691-698
[8]谢婧,徐俐,张秋红,等.顶空固相微萃取法提取菜籽油挥发性风味成分[J].食品科学,2013,34(12):281-285XIE Jing,XU Li,ZHANG Qiu-hong,et al. Headspace solid phase microextraction of volatile flavor components from rapeseed oil[J].Food Science,2013,34(12):281-285
[9]秦早,杨冉,高桂园,等.顶空固相微萃取结合气质联用分析芝麻油和芝麻香精的挥发性成分[J].食品科学,2012,33(24):263-268QIN Zao, YANG Ran,GAO Gui-yuan,et al. Determination of volatile compounds in sesame oil and sesame flavor using headspace solid-phase microextraction and GC-MS[J].Food Science, 2012,33(24):263-268
[10]ZHU Hanjiang, TANG Shuaikun, Charles F. Shoemaker, et al. Characterization of Volatile Compounds of Virgin Olive Oil Originating from the USA[J]. Journal of the American Oil Chemists'Society,2015,92(1):77-85
[11] Giuseppe Procida, Angelo Cichelli, Dario Compagnone et al.Influence of chemical composition of olive oil on the development of volatile compounds during frying[J]. European Food Research and Technology,2009,230(2):217-229
[12]钟诚,薛雅琳,王兴国,等.初榨橄榄油挥发性风味成分的鉴定[J].中国粮油学报,2014,29(12):77-82ZHONG Cheng,XUE Yalin,WANG Xingguo, et al. Identification of Volatile Flavor Components of Virgin Olive Oi[J]. Journal of the Chinese Cereals and Oils Association,2014,29(12):77-82
[13]李芳.热脱附/气相色谱法测定室内空气中TVOC的条件优化[J].山西科技,2015,30(4):93-94LI Fang. The Optimization of the Conditions of Measuring the TVOC(Total Volatile Organic Compound)in the Room Air by Using the Thermal Desorption/Gas Chromatographic Method[J]. Shanxi Science and Technology,2015,30(4):93-94
[14]杜学伟,王锴,杜光尧,等.热脱附/冷阱聚焦/气相色谱/质谱法卷烟香气分析[J].分析测试技术与仪器,2007,13(1):33-40DU Xuewei, WANG Kai, DU Guangyao, et al. Direct thermal desorption-cooled injection System-GC/MS analysis of flavor compounds in cigarette[J]. Analysis and Testing Technology and Instruments,2007,13(1):33-40
[15]高群英,高岩,张汝民,等.3种菊科植物香气成分的热脱附气质联用分析[J].浙江农林大学学报,2011,28(2):326-332GAO Qunying,GAO Yan,ZHANG Rumin, et al. Aromatic composition in three plant species using TDS-GC/MS[J].Journal of Zhejiang Forestry College,2011,28(2):326-332
[16]田怀香,王璋.热脱附-气质联用分析金华火腿挥发性风味[J].食品与机械,2007,23(3):10-13TIAN Huaixiang, WANG Zhang. Theuse of thermal desorption-GC-MS in volatile flavor profiling of jinhua ham[J].Food and Machinery, 2007,23(3):10-13
[17] KALUA C M, BEDGOOD D R, PRENZLER P D. Development of a headspace solid phase microextraction-gas chromatography method for monitoring volatile compounds in extended time-course experiments of olive oil[J]. Analytica Chimica Acta,2006, 556(2):407-414
[18] KALUA C M, ALLEN M S, BEDGOOD J. Olive oil volatile compounds, flavour development and quality:A critical review[J].Food Chemistry,2007,100:273-286
[19] VICHI S,PIZZALE L,CONTE L S. Solid-phase microextraction in the analysis of virgin olive oil volatile fraction:modification induced by oxidation and suitable markers of oxidative status[J]. Agricultural and Food Chemistry,2003,51:6564-6571
[20]向春蓉,徐洲,王寒冬,等.凉山州4个引进品种初榨橄榄油的品质分析[J].中国油脂,2017(3):144-147XIANG Chunrong, XU Zhou, WANG Handong, et al. Quality analysis of virgin olive oils from four introduced varieties in Liangshan[J]. China Oils and Fats, 2017(3):144-147
[21]PROCIDA G, GIOMO A, CICHELLI A,et al. Study of volatile compounds of detective virgin olive oils and sensory evaluation:Achemometric approach[J]. Science of Food and Agriculture, 2005,85:2175-2183
[22] MORALES M T, RIOS J J,APARICIA R. Changes in the volatile composition of virgin olive oil during oxidation:Flavors and off-flavors[J]. Agricultural and Food Chemistry,1997,45:2666-2673.