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顶空固相微萃取-气相色谱-质谱联用法优化与‘安梨’花序挥发性成分分析
引用本文:李晓颍,张文静,刘宝丽,路鑫鑫,赵琦,卢新元,朱京涛.顶空固相微萃取-气相色谱-质谱联用法优化与‘安梨’花序挥发性成分分析[J].中国果树,2020(2):16-22.
作者姓名:李晓颍  张文静  刘宝丽  路鑫鑫  赵琦  卢新元  朱京涛
作者单位:河北科技师范学院园艺科技学院;北省燕山农业特色产业技术研究院;河北省天然产物研究重点实验室(筹)
基金项目:河北省科技厅项目(16236802D-3)。
摘    要:以’安梨’盛花期完整花序为试材,采用顶空固相微萃取-气相色谱-质谱联用技术-(HS-SPME-GC-MS)对其挥发性成分进行分析,通过单因素试验方法对挥发性成分测定条件进行优化,最终确定样品量为3 g,平衡时间与萃取时间均为40 min,萃取温度50 t为最佳测定条件。利用自动质谱解卷积鉴定系统(AMDIS)、NIST11谱库检索系统进行鉴定,在'安梨'花序中共鉴定出61种挥发性成分,包括烷类(26种)、酯类(9种)、醇类(8种)、醛类(6种)、醚类(2种)、萜类(2种)、酮类(2种)、烯类(2种)、芳香类(1种)、酚类(1种)、醞类(1种)、杂环类(1种)以3-辛醇作为内标物对挥发性化合物的含量进行了测定,其中苯醞(8.6μg/kg)、十五烷(5.51μg/kg)、二十一饶(4.42μg/kg)、苯乙醇(4.12μg/kg)、香叶基芳樟醇(2.79 pg/kg)、对苯二酚(2.58 pg/kg)、正十六烷(2.34μgkg)、苯甲醛(1.76μg/kg)等,在’安梨'花序挥发性成分中占有重要比重,是'安梨'花序的主要挥发性成分。由香气品质可知,除烷桂外其他挥发物多具有香气特征,主要表现为花香型、果香型〈青香型、果仁香型、橘香型、苦感型、辛香型和少数其他香型。其中,中级香气品质的挥发物18种,高级香气品质6种。同时,香气系列分布情况也表明,辛香型和花香型是'安梨'花序的主要香气特征,且具有一定程度的果仁香型,与实际嗅感表现一致。

关 键 词:'安梨’    挥发性成分  条件优化  香气品质  顶空固相微萃取-气相色谱-质谱联用技术

Optimization and analysis of aroma components in ‘Anli’ pear flower by headspace solid phase micro-extraction-gas chromatography-mass spectrometry
LI Xiaoying,ZHANG Wenjing,LIU Baoli,LU Xinxin,ZHAO Qi,LU Xinyuan,ZHU Jingtao.Optimization and analysis of aroma components in ‘Anli’ pear flower by headspace solid phase micro-extraction-gas chromatography-mass spectrometry[J].China Fruits,2020(2):16-22.
Authors:LI Xiaoying  ZHANG Wenjing  LIU Baoli  LU Xinxin  ZHAO Qi  LU Xinyuan  ZHU Jingtao
Institution:(College of Horticulture Science&Technology,Hebei Normal University of Science&Technology,Qinhuangdao 066004;Hebei Yanshan Agricultural Characteristic Industry Technology Research Institute;Hebei Provincial Key Laboratory of Active Components and Functions in Natural Products(under planning))
Abstract:The full-bloom stage ‘Anli’ pear flowers were used as experiment materials, and the volatile components were analyzed using headspace solid phase microextraction coupled with gas chromatography-mass spectrometry(HS-SPME-GC-MS), and the determination conditions were optimized by single factor test. The final results shown the optimum condition were sample loading as 3 g, equilibrium and extraction time both as 40 min, and the extraction temperature as 50 ℃. Total of 61 aroma components were detected in the ‘Anli’ pear flower, including 26 alkanes, 9 esters, 8 alcohols, 6 aldehydes, 2 ethers, 2 terpenes, 2 ketones, 2 alkenes, 1 aromatic hydrocarbon, 1 phenol, 1 quinone, and 1 heterocyclic were identified by using the Automatic Mass Spectral Deconvolution and Identification System(AMDIS) and NIST11 mass spectrum database. The 3-octanol was used as internal standard to calculate the content, the result shows, pbenzoquinone(8.56 μg/kg), pentadecane(5.51 μg/kg), heneicosane(4.42 μg/kg), phenylethyl alcohol(4.12 μg/kg), geranyl linalool(2.79 μg/kg), hydroquinone(2.58 μg/kg), hexadecane(2.34 μg/kg), benzaldehyde(1.76 μg/kg), which played an important role in the volatile constituents of ‘Anli’ pear flower. The aroma quality showed that except for alkanes, most volatiles had aroma characteristics, mainly performanced as floral, fruity, green, nutty, citrus, bitter, pungent and a few other flavor-like, among 18 kinds of volatiles with medium odor strength and 6 kinds with high odor strength. In addition, the aroma distribution indicates that the pungent and floral-like as well as a certain degree of nutty-like were the main aroma characteristics, consistent with the actual smell.
Keywords:'Anli'  flower  volatile components  optimum conditions  aroma quality  HS-SPME-GC-MS
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