HS-GC-O-MS分析细叶韭花易挥发性风味成分
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摘要
采用顶空-气相色谱-质谱联用技术对细叶韭花中易挥发性成分的萃取条件及气相色谱-质谱分离检测条件进行系统研究,并结合嗅闻仪确定挥发性风味成分。在选定HP-5MS色谱柱的分离条件下,最优顶空条件为样品用量1.0 g/20.0 mL顶空瓶,平衡温度100℃,平衡时间40 min。结果表明:经气相色谱-嗅闻-质谱联用分析,共分离得到52种化合物,确定结构46种,占总易挥发性成分的99.15%。其中,含硫类17种、醛类10种、烃类4种、酮类4种、呋喃类3种、醇类4种、酸类2种、芳香族类1种、萜类1种。根据嗅闻结果结合相对气味活度值可得,细叶韭花挥发性风味成分主要是二甲基硫醚、二甲基二硫醚、二甲基三硫醚、3-甲基丁醛、2-甲基丁醛、1,3-二噻烷。
The extraction and gas chromatography-mass spectrometry(GC-MS) conditions for analysis of volatile flavor compounds in Allium tenuissimum flowers were systematically studied. An HP-5MS chromatographic column was chosen and the optimal conditions were determined. In this investigation, 1.0 g of sample was extracted at 100 ℃ for 40 min in a 20-mL headspace vial. Under these conditions, a total of 52 compounds were isolated by headspace-gas chromatographyolfactometry-mass spectrometry(HS-GC-O-MS), of which 46 accounting for 99.15% of the total volatile substances, were structurally identified. These compounds included 17 sulfurs, 10 aldehydes, 4 hydrocarbons, 4 ketones, 3 furans, 4 alcohols, 2 acids, 1 aromatic compound, and 1 terpenoid compound. According to the result of olfactometry and relative odor activity value(ROAV), the main flavor volatile components were identified as dimethyl sulfide, 2-methyl-,disulfide, dimethyl trisulfide, 3-methyl-,butanal, 2-methyl,butanal, and 1,3-dithiane.
The extraction and gas chromatography-mass spectrometry(GC-MS) conditions for analysis of volatile flavor compounds in Allium tenuissimum flowers were systematically studied. An HP-5MS chromatographic column was chosen and the optimal conditions were determined. In this investigation, 1.0 g of sample was extracted at 100 ℃ for 40 min in a 20-mL headspace vial. Under these conditions, a total of 52 compounds were isolated by headspace-gas chromatographyolfactometry-mass spectrometry(HS-GC-O-MS), of which 46 accounting for 99.15% of the total volatile substances, were structurally identified. These compounds included 17 sulfurs, 10 aldehydes, 4 hydrocarbons, 4 ketones, 3 furans, 4 alcohols, 2 acids, 1 aromatic compound, and 1 terpenoid compound. According to the result of olfactometry and relative odor activity value(ROAV), the main flavor volatile components were identified as dimethyl sulfide, 2-methyl-,disulfide, dimethyl trisulfide, 3-methyl-,butanal, 2-methyl,butanal, and 1,3-dithiane.
引文
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[19]杨帅,杨文文,胡金芳,等.G C-M S结合保留指数分析白花蛇舌草挥发性成分[J].中国实验方剂学杂志,2012,18(9):93-95.DOI:10.3969/j.issn.1005-9903.2012.09.028.
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[22]孙洁雯,杨克玉,李燕敏.SDE结合GC-MS分析王致和臭豆腐中的特征香气成分[J].食品科学,2015,36(16):127-131.DOI:10.7506/spkx1002-6630-201516023.
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[24]孙培培,黄明泉,孙宝国.同时蒸馏萃取-气质联机分析燕麦片挥发性成分的研究[J].食品工业科技,2011,32(12):479-483.
[25]LRI&odour database[EB/OL].http://www.odour.org.uk/.
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[27]傅润泽,沈建,王锡昌.底播虾夷扇贝活品流通前后挥发性成分的对比分析[J].食品科学,2015,36(2):110-113.DOI:10.7506/spkx1002-6630-201502021.
[28]王武,吴巧,董琪.加工条件对烤制鹌鹑蛋挥发性风味物质的影响[J].食品科学,2013,34(22):234-238.DOI:10.7506/spkx1002-6630-201322046.
[29]李梁.硫醚的合成分析及工艺提纯[J].广州化工,2013,41(15):103-105.DOI:10.3969/j.issn.1001-9677.2013.15.040.
[30]王春燕.甲硫醇合成二甲基二硫醚反应动力学研究与反应器设计[D].重庆:重庆大学,2014.
[31]陈海涛,綦艳梅,徐晓兰,等.月盛斋清香牛肉挥发性成分的分析[J].食品科学,2013,34(18):158-164.DOI:10.7506/spkx1002-6630-201318032.
[32]冯少龙.大蒜提取物中有机硫化物对阪崎克罗诺杆菌的抑菌活性与抑菌机理的研究[D].天津:天津科技大学,2014.
[33]RAJASEKARAN R,KUAN H L,LEE Y S.Recent research progress on garlic(dàsuàn)as a potential anticarcinogenic agent against major digestive cancers[J].Journal of Traditional and Complementary Medicine,2011,2(3):192-201.
[2]栗利元,张未芳,张素珍,等.细叶韭一年实生苗发育节律生物学特性研究[J].黑龙江农业科学,2011(5):68-70.DOI:10.3969/j.issn.1002-2767.2011.05.025.
[3]栗利元,张未芳,郑联寿.细叶韭生活习性的研究[J].黑龙江农业科学,2011(2):63-65.DOI:10.3969/j.issn.1002-2767.2011.02.022.
[4]刘建文.葱属四种植物物候期观测及不同生育期营养成分的研究[D].呼和浩特:内蒙古农业大学,2009.
[5]栗利元,张未芳.细叶韭调味品的产业化初探[J].黑龙江农业科学,2011(9):104-105.DOI:10.3969/j.issn.1002-2767-2011.09.034.
[6]邹总梅,于得泉,丛浦珠,等.葱属植物化学及药理研究进展[J].药学学报,1999,34(5):395-400.DOI:10.3321/j.issn:0513-4870-1999.05.019.
[7]穆启运.细叶韭花化学成分的研究[J].西北植物学报,2001,21(6):1204-1208.DOI:10.3321/j.issn:1000-4025.2001.06.023.
[8]张小利,刘烈淼.超临界C O2提取细叶韭花香精油的工艺研究[J].中国调味品,2012,37(8):74-78.DOI:10.3969/j.issn.1000-9973.2012.08.020.
[9]夏玲君,宋焕禄.香味检测技术GC/O的应用[J].食品与发酵工业,2006,32(1):83-87.DOI:10.3321/j.issn:0253-990X.2006.01.020.
[10]廖远熹,王皓阳,郭寅龙,等.中药柴胡挥发性成分的静态顶空-气相色谱-质谱分析[J].质谱学报,2005,26(3):187-192.DOI:10.3969/j.issn.1004-2997.2005.03.013.
[11]ZHANG Fang,WANG Haoyang,ZHANG Li,et al.Suspected-target pesticide screening using gas chromatography-quadrupole time-offlight mass spectrometry with high resolution deconvolution and retention index/mass spectrum library[J].Talanta,2014,128:156-163.DOI:10.1016/j.talanta.2014.04.068.
[12]孙宝国.食用调香术[M].北京:化学工业出版社,2010:63-350.
[13]许刚,丁浩宸,张燕平,等.南极磷虾头胸部和腹部挥发性风味成分对比[J].食品科学,2014,35(22):146-189.DOI:10.7506/spkx1002-6630-201422027.
[14]刘登勇,周光宏,徐幸莲.确定食品关键风味化合物的一种新方法“ROAV”法[J].食品科学,2008,29(7):370-374.
[15]YUJI Y,YOSHITAKA M,YOSHINORI S,et al.Characterisation of volatile sulphur-containing compounds generated in crushed leaves of Chinese chive(Allium tuberosum Rottler)[J].Food Chemistry,2010,120(2):343-348.DOI:10.1016/j.foodchem.2009.11.028.
[16]HUANG Yonghong,MAO Zhenchuan,XIE Bingyan.Chinese leek(Allium tuberosum Rottler ex Sprengel)reduced disease symptom caused by root-knot nematode[J].Integrative Agriculture,2016,15(2):364-372.DOI:10.1016/S2095-3119(15)61032-2.
[17]郑福平,孙宝国,刘玉平,等.同时蒸馏萃取气质联机分析腌渍野韭菜花香成分[J].食品科学,2009,30(22):247-249.DOI:10.3321/j.issn:1002-6630.2009.22.056.
[18]王呈仲,苏越,郭寅龙.顶空-气相色谱-质谱联用分析桂花和叶中挥发性成分[J].有机化学,2009,29(6):948-955.
[19]杨帅,杨文文,胡金芳,等.G C-M S结合保留指数分析白花蛇舌草挥发性成分[J].中国实验方剂学杂志,2012,18(9):93-95.DOI:10.3969/j.issn.1005-9903.2012.09.028.
[20]刘朋,徐琳琳,吕青涛,等.顶空进样GC-MS结合保留指数分析补骨脂挥发性成分[J].中国实验方剂杂志,2011,17(10):74-76.DOI:10.3969/j.issn.1005-9903.2011.10.023.
[21]孙洁雯,杨克玉,李燕敏.东北特产许氏大酱中挥发性成分的提取与分析[J].食品研究与开发,2015,36(14):115-120.DOI:10.3969/j.issn.1005-6521.2015.14.029.
[22]孙洁雯,杨克玉,李燕敏.SDE结合GC-MS分析王致和臭豆腐中的特征香气成分[J].食品科学,2015,36(16):127-131.DOI:10.7506/spkx1002-6630-201516023.
[23]CLARA C C,DIANA G P,VEGA,et al.Novel approach for the determination of volatile compounds in processed onion by headspace gas chromatography-mass spectrometry(HS GC-MS)[J].Talanta,2013,103:137-144.DOI:10.1016/j.talanta.2012.10.022.
[24]孙培培,黄明泉,孙宝国.同时蒸馏萃取-气质联机分析燕麦片挥发性成分的研究[J].食品工业科技,2011,32(12):479-483.
[25]LRI&odour database[EB/OL].http://www.odour.org.uk/.
[26]孙颖,陈怡颖,丁奇,等.小根蒜挥发性风味成分分析[J].食品科学,2015,36(16):117-121.DOI:10.7506/spkx1002-6630-201516021.
[27]傅润泽,沈建,王锡昌.底播虾夷扇贝活品流通前后挥发性成分的对比分析[J].食品科学,2015,36(2):110-113.DOI:10.7506/spkx1002-6630-201502021.
[28]王武,吴巧,董琪.加工条件对烤制鹌鹑蛋挥发性风味物质的影响[J].食品科学,2013,34(22):234-238.DOI:10.7506/spkx1002-6630-201322046.
[29]李梁.硫醚的合成分析及工艺提纯[J].广州化工,2013,41(15):103-105.DOI:10.3969/j.issn.1001-9677.2013.15.040.
[30]王春燕.甲硫醇合成二甲基二硫醚反应动力学研究与反应器设计[D].重庆:重庆大学,2014.
[31]陈海涛,綦艳梅,徐晓兰,等.月盛斋清香牛肉挥发性成分的分析[J].食品科学,2013,34(18):158-164.DOI:10.7506/spkx1002-6630-201318032.
[32]冯少龙.大蒜提取物中有机硫化物对阪崎克罗诺杆菌的抑菌活性与抑菌机理的研究[D].天津:天津科技大学,2014.
[33]RAJASEKARAN R,KUAN H L,LEE Y S.Recent research progress on garlic(dàsuàn)as a potential anticarcinogenic agent against major digestive cancers[J].Journal of Traditional and Complementary Medicine,2011,2(3):192-201.
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