肖云龙,从艳霞,明守安,涂行浩,张维农,吴宗远

• 1:武汉轻工大学食品科学与工程学院
• 2:农产品加工与转化湖北省重点实验室
• 3:大宗粮油精深加工教育部重点实验室
• 4:湖北明创农业科技发展有限公司

摘要(Abstract)：

花椒叶生长周期短、可再生性强，具有广阔的开发应用前景。为了全面解析花椒叶精油的关键香气成分，该研究首先通过单因素实验和正交实验对花椒叶精油的提取工艺以及后续GC-MS分析的前处理条件进行了优化。结果显示，水蒸气蒸馏法提取花椒叶精油的最佳工艺条件为未粉碎、料液比1∶6、提取时间5 h;溶剂萃取法提取花椒叶精油的最佳工艺条件为粉碎度40目、料液比1∶7、提取时间3 h。同时，确定SPME为色谱分析前处理的最佳方法。随后，采用HS-SPME-GC-MS法和感官评价对优化条件下获得的花椒叶精油成分进行分析，并通过计算气味活度值(OAV)筛选出关键香气成分(OAV≥1)。研究发现，SD法提取的精油共检测到8种关键香气成分，而SE法提取的精油仅检测到1种。该研究为花椒叶精油的质量评价提供了潜在的关键香气成分。

关键词(KeyWords)： 花椒叶精油;蒸馏法;溶剂萃取法;关键香气成分

Abstract:

Keywords:

基金项目(Foundation): 武汉轻工大学引进人才科研启动项目(2025RZ010);; 大宗粮油精深加工省部共建教育部重点实验室开放课题(DZLY2023005);; 中央引导地方科技发展专项项目(2022BGE247)

作者(Author): 肖云龙,从艳霞,明守安,涂行浩,张维农,吴宗远

参考文献(References)：

• [1]MENG F B,LEI Y T,ZHANG Q,et al.Encapsulation of Zanthoxylum bungeanum essential oil to enhance flavor stability and inhibit lipid oxidation of Chinese-style sausage[J].Journal of the Science of Food and Agriculture,2022,102(10):4035-4045.
• [2]KHARRAF S E,EL-GUENDOUZ S,FARAH A,et al.Hydrodistillation and simultaneous hydrodistillation-steam distillation of Rosmarinus officinalis and Origanum compactum:antioxidant,anti-inflammatory,and antibacterial effect of the essential oils[J].Industrial Crops and Products,2021,168:113591.
• [3]姚丽.我国花椒加工技术研究进展[J].食品安全质量检测学报,2024,15(15):127-135.
• [4]SHARMA S,BARKAUSKAITE S,JAISWAL K,et al.Essential oils as additives in active food packaging[J].Food Chemistry,2021,343:128403.
• [5]李春丽.花椒中的化学成分及其生物活性的研究[D].兰州:西北民族大学,2021.
• [6]吴文博.胃寒吃点花椒叶消宿食温脾胃[J].家庭医药·快乐养生,2017(5):41.
• [7]LOCALI-PEREIRA R,LOPES N A,MENIS-HENRIQUE MC,et al.Modulation of volatile release and antimicrobial properties of pink pepper essential oil by microencapsulation in single-and double-layer structured matrices[J].International Journal of Food Microbiology,2020,335:108890.
• [8]JARADAT N.Qualitative and quantitative comparison of aromatic oil components and antifungal effects of Cymbopogon flexuosus obtained with supercritical CO2,microwave-ultrasonic,steam distillation,and hydrodistillation extraction techniques[J].Molecules,2023,28(19):6870.
• [9]LIU Y,SU H,SONG L.Comparison of four extraction methods,SPME,DHS,SAFE,versus SDE,for the analysis of flavor compounds in natto[J].Food Analytical Methods,2018,11(2):343-354.
• [10]XUE J,GUO G Y,LIU P P,et al.Identification of aromaactive compounds responsible for the floral and sweet odors of Congou black teas using gas chromatography-mass spectrometry/olfactometry,odor activity value,and chemometrics[J].Journal of the Science of Food and Agriculture,2022,102(12):5399-5410.
• [11]罗凯,朱琳,阚建全.水蒸汽蒸馏、溶剂萃取、同时蒸馏萃取法提取花椒挥发油的效果比较[J].食品科技,2012,37(10):234-236,240.
• [12]赵志峰,覃哲,雷绍荣.三种花椒精油的提取研究[J].食品工业科技,2007(12):143-144,147.
• [13]里奥·范海默特.化合物嗅觉阈值汇编(原书第二版)[M].李智宇,译.北京:科学出版社,2018:242-645.
• [14]NI J,WANG X,SHEN Y,et al.Recent updates on the chemistry,bioactivities,mode of action,and industrial applications of plant essential oils[J].Trends in Food Science Technology,2021,110:78-89.
• [15]CHUO C,NASIR H M,MOHD-SETAPAR S H,et al.Aglimpse into the extraction methods of active compounds from plants[J].Critical Reviews in Analytical Chemistry,2022,52(4):667-696.
• [16]VIAN A,FERNANDEZ X,VISINONI F,et al.Microwave hydrodiffusion and gravity,new technique for extraction of essential oils[J].Journal of Chromatography A,2008,1190(1-2):14-17.
• [17]TONGNUANCHAN P,BENJAKUL S.Essential oils:extraction,bioactivities,and their uses for food preservation[J].Food Science,2014,79(7):1231-1249.
• [18]GAO C,CHEN S,JIN G Y,et al.Solvent effects and mass transfer on aroma extraction during solid-state distillation[J].Food Bioscience,2023,53:102682.
• [19]孙丰义,王丹,陈海涛,等.SPME和SAFE对比分析炸花椒油挥发性风味成分[J].精细化工,2016,33(1):49-54,61.
• [20]白亚蒙,张峰升,李皓,等.基于GC-MS对顶空固相萃取法和微波辅助法获得的花椒挥发油香气成分分析[J].中国调味品,2023,48(3):187-190.
• [21]WANG L,ZHU C,WANG Y Q,et al.Characterization of aroma-impact compounds in dry jujubes (Ziziphus jujube Mill.) by aroma extract dilution analysis (AEDA) and gas chromatography-mass spectrometer (GC-MS)[J].International Journal of Food Properties,2018,21(1):1844-1853.
• [22]JI Y,LI M,HO C T.Chemical composition,sensory properties and application of Sichuan pepper (Zanthoxylum genus)[J].Food Science and Human Wellness,2019,8(2):115-125.
• [23]陈茜,陶兴宝,黄永亮,等.花椒香气研究进展[J].中国调味品,2018,43(1):189-194.
• [24]周敏,刘福权,吕远平,等.花椒的超临界CO2萃取和水蒸气蒸馏工艺对比研究[J].中国调味品,2022,47(8):101-105.
• [25]周琦,谈安群,欧阳祝,等.橙汁与宽皮橘汁关键香气的比较及其在各自主体风味呈现中的作用[J].食品与发酵工业,2021,47(21):259-267.
• [26]MOLLICA F,GELABERT I,AMORATI R.Synergic antioxidant effects of the essential oil component γ-terpinene on hightemperature oil oxidation[J].ACS Food Science Technology,2022,2(1):180-186.
• [27]SEPTIANA S,YULIANA D,BACHTIAR B M,et al.Metabolomics approach for determining potential metabolites correlated with sensory attributes of Melaleuca cajuputi essential oil,promising flavor ingredient[J].Journal of Bioscience and Bioengineering,2020,129(5):581-587.
• [28]CHIGO-HERNANDEZ M,DUBOIS A,TOMASINO E.Aroma perception of rose oxide,linalool and α-terpineol combinations in Gewürztraminer wine[J].Foods,2022,8(1):30.
• [29]GUO Y,ADELINA N M,HU J T,et al.Comparative analysis of volatile profiles in four pine-mushrooms using HS-SPME/GC-MS and E-nose[J].Food Control,2022,134:108711.
• [30]NIU J,TIAN H L,ZHAN P.The effects of pepper(Zanthoxylum bungeanum) from different production areas on the volatile flavor compounds of fried pepper oils based on HS-SPME-GC-MS and multivariate statistical method[J].Molecules,2022,27(22):7760.
• [31]THIBAUD F,COURREGELONGUE M,DARRIET P.Contribution of volatile odorous terpenoid compounds to aged cognac spirits aroma in context of multicomponent odor mixtures[J].Journal of Agricultural and Food Chemistry,2020,68(47):13310-13318.
• [32]NI J,YAN H Y,TIAN H L,et al.Characterization of key odorants in fried red and green Huajiao (Zanthoxylum bungeanum Maxim.and Zanthoxylum schinifolium sieb.et Zucc.) oils[J].Food Chemistry,2022,377:131984.
• [33]WANG V,JING S,WANG X L,et al.Evaluation of the perceptual interaction among ester odorants and nonvolatile organic acids in Baijiu by GC-MS,GC-O,odor threshold,and sensory analysis[J].Journal of Agricultural and Food Chemistry,2022,70(43):13987-13995.
• [34]GON??ALVES D,COSTA P,BEJAR L,et al.Air diffusion of aroma-active components from crude citrus essential oils and their extract phases obtained by solvent extraction[J].Industrial Engineering Chemistry Research,2018,57(16):5670-5679.
• [35]马钤,郭川川,张峰轶,等.花椒精油亚临界流体萃取工艺优化及GC-MS分析[J].中国酿造,2022,41(10):201-206.
• [36]FIDYT K,FIEDOROWICZ A,STRZ DA??A L,et al.β-caryophyllene and β-caryophyllene oxide-natural compounds of anticancer and analgesic properties[J].Cancer Medicine,2016,5(10):3007-3017.
• [37]BHATTACHARYA R,SHARMA P,BOSE D,et al.Synergistic potential of α-phellandrene combined with conventional antifungal agents and its mechanism against antibiotic resistant Candida albicans[J].CABI Agriculture and Bioscience,2024,5(1):17.
• [38]LAZAREVIC J,ACIMOVIC M,-DUROVIC-PEJCEV R,et al.Linking weed control techniques to anti-inflammatory potential:comparative analysis of Angelica archangelica L.root essential oil profiles[J].Industrial Crops and Products,2024,216:118656.
• [39]BALDISSERA D,GRANDO T H,SOUZA C F,et al.In vitro and in vivo action of terpinen-4-ol,γ-terpinene,and α-terpinene against Trypanosoma evansi[J].Experimental Parasitology,2016,162:43-48.
• [40]NARARAK J,SATHANTRIPHOP S,KONGMEE M,et al.Excito-repellent activity of β-caryophyllene oxide against Aedes aegypti and Anopheles minimus[J].Acta Tropica,2019,197:105030.
• [41]QUIROGA R,NEPOTE V,BAUMGARTNER M T.Contribution of organic acids to α-terpinene antioxidant activity[J].Food Chemistry,2019,277:267-272.
• [42]ERYIGIT T,YILDIRIM B,EKICI K,et al.Chemical composition,antimicrobial and antioxidant properties of Schinus molle L.essential oil from turkey[J].Journal of Essential Oil Bearing Plants,2017,20(2):570-577.