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3种不同萃取方法对黑胡椒香气物质的气质联用分析
引用本文:王珏,钟壹鸣,孙也乔,胡丽松,伍宝朵,郝朝运,范睿.3种不同萃取方法对黑胡椒香气物质的气质联用分析[J].热带作物学报,2022,43(5):1055-1063.
作者姓名:王珏  钟壹鸣  孙也乔  胡丽松  伍宝朵  郝朝运  范睿
作者单位:1.海南大学热带作物学院,海南海口 5702282.中国热带农业科学院香料饮料研究所,海南万宁 5715333.海南省遗传育种与种质资源重点实验室,海南万宁 5715334.海南省热带香辛饮料作物遗传改良与品质调控重点实验室,海南万宁 5715335.海南省Sim Soonliang院士工作站,海南万宁 571533
基金项目:香料饮料种质圃安全保存基金项目;财政部和农业农村部国家现代农业产业技术体系资助项目(CARS-11);海南省院士创新平台科研专项(YSPTZX202154)
摘    要:为探究不同提取方法对黑胡椒挥发性成分的影响,本研究以黑胡椒为材料,利用顶空固相微萃取法(HS-SPME)、戊烷:乙醚(1:1)溶剂萃取法和甲基叔丁基醚(MTBE)溶剂萃取法对黑胡椒中的香气成分进行提取,结合气相色谱质谱联用法(gas chromatography-mass spectrometry)和主成分分析法(PCA)对提取的香气物质进行分析。3种提取方法共得到6类(烯类、醇类、酚类、烃类、崁类、烯类氧化物)33种物质。戊烷:乙醚(1:1)溶剂萃取法、MTBE溶剂萃取法及顶空固相微萃取法分别检测到25、23、27种挥发性化合物,其中,相对含量较高的化合物均为3-蒈烯、柠檬烯、β-石竹烯、β-蒎烯。2种溶剂萃取法中,戊烷:乙醚(1:1)溶剂萃取法检测到的特有化合物有α-松油烯、α-松油醇、β-金合欢烯;与2种溶剂萃取法相比,顶空固相微萃取法(HS-SPME)检测到的特有化合物有樟脑、4-萜烯醇、2-(4-甲基苯基)丙-2-醇、橙花醇、香树烯、β-甜没药烯和愈创兰油烃。结合主成分分析得出,β-蒎烯、3-蒈烯、柠檬烯、β-石竹烯对黑胡椒香气风味贡献率较大,其中顶空固相微萃取法(HS-SPME)与2种溶剂萃取法所得成分差异明显。在溶剂萃取法中,戊烷:乙醚(1:1)溶剂萃取法优于MTBE溶剂萃取法。溶剂萃取法与顶空固相微萃取法所得物质在种类与数量上均存在差异。在胡椒香气物质检测时,将2种方法相结合可以更大程度保证所得化合物种类的丰富性和全面性。

关 键 词:黑胡椒  溶剂萃取  顶空固相微萃取  气质联用  
收稿时间:2021-11-23

Analysis of Aroma Substances in Black Pepper by Three Different Extraction Methods by GC-MS
WANG Jue,ZHONG Yiming,SUN Yeqiao,HU Lisong,WU Baoduo,HAO Chaoyun,FAN Rui.Analysis of Aroma Substances in Black Pepper by Three Different Extraction Methods by GC-MS[J].Chinese Journal of Tropical Crops,2022,43(5):1055-1063.
Authors:WANG Jue  ZHONG Yiming  SUN Yeqiao  HU Lisong  WU Baoduo  HAO Chaoyun  FAN Rui
Abstract:The study was aimed to explore the effects of different extraction methods on the volatile components of black pepper. Using black pepper as the material, headspace solid phase microextraction (HS-SPME), pentane:diethyl ether (1:1) solvent extraction and MTBE solvent extraction were used to extract the aroma components in black pepper, and gas chromatography-mass spectrometry combined with principal component analysis (PCA) was used to analyze the extracted aroma substances. A total of 33 substances in 6 categories (alkenes, alcohols, phenols, hydrocarbons, olefins, and olefin oxides) were obtained under the three extraction methods. 25, 23, 27 volatile compounds were respectively detected in the pentane:diethyl ether (1:1) solvent extraction method, MTBE solvent extraction method and headspace solid phase microextraction method. The compounds with relatively high content of volatile compounds obtained by the three extraction methods were 3-carene, limonene, β-caryophyllene, and β-pinene. α-terpinene, α-terpineol, β-farnesene were only detected in the pentane:diethyl ether (1:1) solvent extraction method. Camphor, 4-terpene alcohol, 2-(4-methylphenyl) propan-2-ol, and nerol, alloaromadendrene, β-Bisabolene and guaiazulene were only found in HS-SPME. Combined with principal component analysis (PCA), β-pinene, 3-carene, limonene, and β-caryophyllene contributed significantly to the aroma and flavor of black pepper. Among them, the composition of HS-SPME and the two solvent extraction methods were significantly different. In the solvent extraction methods, the pentane:diethyl ether (1:1) solvent extraction method was better than the MTBE solvent extraction method, and there were differences in the types and quantities of substances obtained by the solvent extraction method and the headspace solid phase microextraction method. In the detection of pepper aroma substances, the combination of the two methods could ensure the richness and comprehensiveness of the obtained compounds to a greater extent.
Keywords:black pepper  solvent extraction  headspace solid phase microextraction  gas chromatography-mass spectrometry  
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