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Article(id=1320880758223389403, tenantId=1146029695717560320, journalId=1260987677001138203, issueId=1320880625310085394, articleNumber=null, orderNo=null, doi=10.13386/j.issn1002-0306.2025080033, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1754841600000, receivedDateStr=2025-08-11, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1792852113538, onlineDateStr=2026-10-24, pubDate=1788192000000, pubDateStr=2026-09-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792852113538, onlineIssueDateStr=2026-10-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792852113538, creator=13701087609, updateTime=1792852113538, updator=13701087609, issue=Issue{id=1320880625310085394, tenantId=1146029695717560320, journalId=1260987677001138203, year='2026', volume='47', issue='17', pageStart='1', pageEnd='596', issueExtLink='null', onlineDate='null', pubDate='1788192000000', pubDateStr='2026-09-01', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792852081848, creator='13701087609', updateTime=1792852081848, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=368, endPage=376, ext={EN=ArticleExt(id=1320880758454076124, articleId=1320880758223389403, tenantId=1146029695717560320, journalId=1260987677001138203, language=EN, title=Magnetic Solid-phase Extraction Coupled with Gas Chromatography-Mass Spectrometry for Efficient Analysis of 1,1,6-Trimethyl-1,2-dihydronaphthalene in Wine, columnId=1261343843585241413, journalTitle=Science and Technology of Food Industry, columnName=Analysis and Determination, runingTitle=null, highlight=null, articleAbstract=

This study aimed to establish a novel and efficient analytical method based on magnetic expanded graphite (MEG) solid-phase extraction coupled with gas chromatography-mass spectrometry to address the challenge of accurately determining the trace characteristics of the aroma compound 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) in Riesling wines. The MEG adsorbent was prepared via a facile physical blending method, and its physicochemical properties were systematically characterized. Additionally, the key parameters affecting the magnetic solid-phase extraction (MSPE) pretreatment were optimized. Furthermore, density functional theory calculations were employed to investigate the adsorption mechanism at the molecular level. The results indicated that the method exhibited good linearity in the range of 0.05~100 ng/mL (R2=0.9943), with a limit of detection as low as 0.01 ng/mL. Theoretical calculations confirmed that the synergistic effect of van der Waals forces and π–π stacking (binding energy: −0.84 eV) was the key driving force for the efficient adsorption of TDN. The proposed method was successfully applied to the analysis of various Riesling wine samples, demonstrating high efficiency, accuracy, and reliability in the quantitative analysis of the target compound. This study not only provides a rapid and sensitive analytical tool for TDN but also offers new insights guided by theoretical calculations for the design and application of novel enrichment materials for food flavor compounds.

, authors=Huihui GAO, Houxin JIN, Hongcun BAI, Haobo ZHENG*, authorsList=Huihui GAO, Houxin JIN, Hongcun BAI, Haobo ZHENG, authorCompany=null, correspAuthors=Haobo ZHENG, authorNote=null, correspAuthorsNote=null, copyrightStatement=Copyright © 2026 Science and Technology of Food Industry. All rights reserved., copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1320880761742410481, articleId=1320880758223389403, tenantId=1146029695717560320, journalId=1260987677001138203, language=CN, title=磁固相萃取-气相色谱-质谱联用法高效分析葡萄酒中1,1,6-三甲基-1,2-二氢萘, columnId=1261343846139572559, journalTitle=食品工业科技, columnName=分析检测, runingTitle=null, highlight=null, articleAbstract=

为解决雷司令葡萄酒中痕量特征香气物质1,1,6-三甲基-1,2-二氢萘（1,1,6-trimethyl-1,2-dihydronaphthalene，TDN）精准测定难题，本研究旨在建立一种基于磁性膨胀石墨（magnetic expanded graphite，MEG）的高效磁固相萃取-气相色谱-质谱联用分析新方法，通过简便的物理共混法制备MEG吸附剂，系统表征其理化性质，并优化了MSPE前处理的关键参数。同时，采用密度泛函理论计算从分子层面探究了吸附机理。结果表明，该方法在0.05~100 ng/mL范围内线性关系良好（R2=0.9943），检出限低至0.01 ng/mL。理论计算证实，范德华力与π–π堆积的协同作用（结合能−0.84 eV）是实现TDN高效吸附的关键驱动力。该方法已成功应用于多种雷司令葡萄酒样品，展现出目标化合物定量分析的高效性、准确性和可靠性。本研究不仅建立了一种快速、灵敏的TDN分析工具，也为基于理论计算指导新型食品风味物质富集材料的设计与应用提供了新思路。

, authors=高慧慧, 靳候鑫, 白红存, 郑浩博*, authorsList=高慧慧, 靳候鑫, 白红存, 郑浩博, authorCompany=null, correspAuthors=郑浩博, authorNote=

高慧慧（1997−），女，硕士研究生，研究方向：分离科学与技术，E-mail：

, correspAuthorsNote=
郑浩博（1989−），男，博士，副教授，研究方向：分离科学与技术，E-mail：。
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高慧慧（1997−），女，硕士研究生，研究方向：分离科学与技术，E-mail：

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高慧慧（1997−），女，硕士研究生，研究方向：分离科学与技术，E-mail：

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Volatile aroma compound-based decoding and prediction of sweet berry aromas in dry red wine[J]. Food Chemistry, 2025, 463: 141248., articleTitle=null, refAbstract=null), Reference(id=1320881000792572631, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=2, rfOrder=1, authorNames=null, journalName=null, refType=null, unstructuredReference=CAFFREY A J, LERNO L A, ZWEIGENBAUM J, et al. Characterization of free and bound monoterpene alcohols during Riesling fermentation[J]. Journal of Agricultural and Food Chemistry, 2021, 69(45): 13286−13298., articleTitle=null, refAbstract=null), Reference(id=1320881000880653016, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=3, rfOrder=2, authorNames=null, journalName=null, refType=null, unstructuredReference=LI L Y. Memory1,1,6-trimethyl-1,2-dihydroxnapthalene (TDN) is a common odor defect of Riesling wine (petrol) that screams "Riesling" at subthreshold levels[D]. New York: Cornell University, 2025., articleTitle=null, refAbstract=null), Reference(id=1320881000947761881, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=4, rfOrder=3, authorNames=null, journalName=null, refType=null, unstructuredReference=HAAG F, FREY T, BALL L, et al. Petrol note in Riesling-1,1, 6-trimethyl-1,2-dihydronaphthalene (TDN) selectively activates human odorant receptor OR8H1[J]. Journal of Agricultural and Food Chemistry, 2024, 72(9): 4888−4896., articleTitle=null, refAbstract=null), Reference(id=1320881002600317659, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=5, rfOrder=4, authorNames=null, journalName=null, refType=null, unstructuredReference=ZIEGLER M, GÖK R, BECHTLOFF P, et al. Impact of matrix variables and expertise of panelists on sensory thresholds of 1,1,6-trimethyl-1,2-dihydronaphthalene known as petrol off-flavor compound in Riesling wines[J]. Food Quality and Preference, 2019, 78: 103735., articleTitle=null, refAbstract=null), Reference(id=1320881002709369564, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=6, rfOrder=5, authorNames=null, journalName=null, refType=null, unstructuredReference=GÖK R, SELHORST P, KIENE M, et al. Target-guided isolation of progenitors of 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) from Riesling wine by high-performance countercurrent chromatography[J]. Molecules, 2022, 27(17): 5378., articleTitle=null, refAbstract=null), Reference(id=1320881002784867037, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=7, rfOrder=6, authorNames=null, journalName=null, refType=null, unstructuredReference=ANTAL E, VARGA Z, KÁLLAY M, et al. 1,1,6-trimethyl-1,2-dihydronaphthalene content of Riesling wines in Hungary[J]. ACS Omega, 2023, 8(40): 36677−36685., articleTitle=null, refAbstract=null), Reference(id=1320881002847781598, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=8, rfOrder=7, authorNames=null, journalName=null, refType=null, unstructuredReference=LESZCZYŃSKA D, HALLMANN A, TREDER N, et al. Recent advances in the use of SPME for drug analysis in clinical, toxicological, and forensic medicine studies[J]. Talanta, 2024, 270: 125613., articleTitle=null, refAbstract=null), Reference(id=1320881002906501855, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=9, rfOrder=8, authorNames=null, journalName=null, refType=null, unstructuredReference=HAO Yaofei, LI Jianxun, ZHAO Zhiheng, et al. Flavor characteristics of Shanlan rice wines fermented for different time based on HS-SPME-GC-MS-O, HS-GC-IMS, and electronic sensory analyses[J]. Food Chemistry, 2024, 432: 137150., articleTitle=null, refAbstract=null), Reference(id=1320881002977805024, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=10, rfOrder=9, authorNames=null, journalName=null, refType=null, unstructuredReference=CASTELL A, ARROYO-MANZANARES N, VIÑAS P, et al. Advanced materials for magnetic solid-phase extraction of mycotoxins: A review[J]. TrAC Trends in Analytical Chemistry, 2024, 178: 117826., articleTitle=null, refAbstract=null), Reference(id=1320881003044913889, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=11, rfOrder=10, authorNames=null, journalName=null, refType=null, unstructuredReference=FU Quanbin, XIA Zhenzhen, SUN Xin, et al. Recent advance and applications of covalent organic frameworks based on magnetic solid-phase extraction technology for food safety analysis[J]. TrAC Trends in Analytical Chemistry, 2023, 162: 117054., articleTitle=null, refAbstract=null), Reference(id=1320881003128799970, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=12, rfOrder=11, authorNames=null, journalName=null, refType=null, unstructuredReference=JAFARI Z, GHANI M. Magnetic carbonized cellulose-MIL 101(Fe) composite as a sorbent for magnetic solid phase extraction of selected organophosphorus pesticides combined with high performance liquid chromatography-ultraviolet detection[J]. Talanta Open, 2023, 7: 100212., articleTitle=null, refAbstract=null), Reference(id=1320881003200103139, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=13, rfOrder=12, authorNames=null, journalName=null, refType=null, unstructuredReference=ZHAO Mingming, WU Haizhi, DENG Xiaoke, et al. The application progress of magnetic solid-phase extraction for heavy metal analysis in food: A mini review[J]. Analytical Methods, 2024, 16(3): 333−343., articleTitle=null, refAbstract=null), Reference(id=1320881003267212004, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=14, rfOrder=13, authorNames=null, journalName=null, refType=null, unstructuredReference=ELBIDI M, MOHD SALLEH M A, RASHID S A, et al. The potential of thermally expanded graphite in oil sorption applications[J]. RSC Advances, 2024, 14(23): 16466−16485., articleTitle=null, refAbstract=null), Reference(id=1320881003346903781, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=15, rfOrder=14, authorNames=null, journalName=null, refType=null, unstructuredReference=SUN Kangkang, LIU Muyu, SUN Kaige, et al. High-efficiently and rapidly capturing cesium from water with Prussian blue@expanded graphite as adsorbent[J]. Journal of Industrial and Engineering Chemistry, 2023, 125: 336−344., articleTitle=null, refAbstract=null), Reference(id=1320881003405624038, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=16, rfOrder=15, authorNames=null, journalName=null, refType=null, unstructuredReference=ZHENG Haobo, DING Jun, ZHENG Shujian, et al. Facile synthesis of magnetic carbon nitride nanosheets and its application in magnetic solid phase extraction for polycyclic aromatic hydrocarbons in edible oil samples[J]. Talanta, 2016, 148: 46−53., articleTitle=null, refAbstract=null), Reference(id=1320881003497898727, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=17, rfOrder=16, authorNames=null, journalName=null, refType=null, unstructuredReference=SACKS G L, GATES M J, FERRY F X, et al. Sensory threshold of 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) and concentrations in young Riesling and non-Riesling wines[J]. Journal of Agricultural and Food Chemistry, 2012, 60(12): 2998−3004., articleTitle=null, refAbstract=null), Reference(id=1320881003573396200, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=18, rfOrder=17, authorNames=null, journalName=null, refType=null, unstructuredReference=LU Tian, CHEN Feiwu. Multiwfn: A multifunctional wavefunction analyzer[J]. Journal of Computational Chemistry, 2012, 33(5): 580−592., articleTitle=null, refAbstract=null), Reference(id=1320881003644699369, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=19, rfOrder=18, authorNames=null, journalName=null, refType=null, unstructuredReference=HUMPHREY W, DALKE A, SCHULTEN K. VMD: Visual molecular dynamics[J]. Journal of Molecular Graphics, 1996, 14(1): 33−38., articleTitle=null, refAbstract=null), Reference(id=1320881003732779754, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=20, rfOrder=19, authorNames=null, journalName=null, refType=null, unstructuredReference=JOHNSON E R, KEINAN S, MORI-SÁNCHEZ P, et al. Revealing noncovalent interactions[J]. Journal of the American Chemical Society, 2010, 132(18): 6498−6506., articleTitle=null, refAbstract=null), Reference(id=1320881003799888619, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=21, rfOrder=20, authorNames=null, journalName=null, refType=null, unstructuredReference=FRISCH M, TRUCKS G, SCHLEGEL H, et al. St: Gaussian 16 revision C. 01[J]. Gaussian Inc, Wallingford CT, 2016., articleTitle=null, refAbstract=null), Reference(id=1320881003892163308, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=22, rfOrder=21, authorNames=null, journalName=null, refType=null, unstructuredReference=ZHENG Haobo, DING Jun, ZHENG Shujian, et al. Magnetic "one-step" quick, easy, cheap, effective, rugged and safe method for the fast determination of pesticide residues in freshly squeezed juice[J]. Journal of Chromatography A, 2015, 1398: 1−10., articleTitle=null, refAbstract=null), Reference(id=1320881003967660781, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=23, rfOrder=22, authorNames=null, journalName=null, refType=null, unstructuredReference=WANG Bin, CHEN Yongyue, LI Wenxuan, et al. Magnetic phytic acid-modified kapok fiber biochar as a novel sorbent for magnetic solid-phase extraction of antidepressants in biofluids[J]. Analytica Chimica Acta, 2024, 1296: 342295., articleTitle=null, refAbstract=null), Reference(id=1320881004043158254, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=24, rfOrder=23, authorNames=null, journalName=null, refType=null, unstructuredReference=HOU Bo, SUN Hongjuan, PENG Tongjiang, et al. Rapid preparation of expanded graphite at low temperature[J]. New Carbon Materials, 2020, 35(3): 262−268., articleTitle=null, refAbstract=null), Reference(id=1320881004135432943, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=25, rfOrder=24, authorNames=null, journalName=null, refType=null, unstructuredReference=ZHANG Kaige, WANG Jing, GUO Rong, et al. Acid induced dispersive liquid-liquid microextraction based on in situ formation of hydrophobic deep eutectic solvents for the extraction of bisphenol A and alkylphenols in water and beverage samples[J]. Food Chemistry, 2024, 442: 138425., articleTitle=null, refAbstract=null), Reference(id=1320881004332565232, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=26, rfOrder=25, authorNames=null, journalName=null, refType=null, unstructuredReference=KARAPıNAR H S, BALıKÇıOĞLU A. Boron-doped activated carbon nanocomposite as a selective adsorbent for rapid extraction of aflatoxins in nut samples[J]. Journal of Food Composition and Analysis, 2022, 112: 104680., articleTitle=null, refAbstract=null), Reference(id=1320881004399674097, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=27, rfOrder=26, authorNames=null, journalName=null, refType=null, unstructuredReference=LI Min, LIU Weihua, MENG Xufeng, et al. Facile synthesis of magnetic hypercrosslinked polymer for the magnetic solid-phase extraction of benzoylurea insecticides from honey and apple juice samples[J]. Food Chemistry, 2022, 395: 133596., articleTitle=null, refAbstract=null), Reference(id=1320881004479365874, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=28, rfOrder=27, authorNames=null, journalName=null, refType=null, unstructuredReference=LU Tian, CHEN Qinxue. Interaction region indicator: A simple real space function clearly revealing both chemical bonds and weak interactions[J]. Chemistry-Methods, 2021, 1(5): 231−239., articleTitle=null, refAbstract=null), Reference(id=1320881004575834867, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=29, rfOrder=28, authorNames=null, journalName=null, refType=null, unstructuredReference=FAN Sheng, LU Xinru, LI Haoliang, et al. Efficient removal of organophosphate esters by ligand functionalized MIL-101 (Fe): Modulated adsorption and DFT calculations[J]. Chemosphere, 2022, 302: 134881., articleTitle=null, refAbstract=null), Reference(id=1320881004655526644, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=30, rfOrder=29, authorNames=null, journalName=null, refType=null, unstructuredReference=WANG Bin, XU Shuangjiao, LI Wenxuan, et al. Polyaniline-coated kapok fibers for convenient in-syringe solid-phase microextraction and determination of organochlorine and pyrethroid pesticide residues in aqueous samples[J]. Talanta, 2024, 271: 125706., articleTitle=null, refAbstract=null), Reference(id=1320881004731024117, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=31, rfOrder=30, authorNames=null, journalName=null, refType=null, unstructuredReference=ZIEGLER M, WEGMANN-HERR P, SCHMARR H G, et al. Impact of rootstock, clonal selection, and berry size of Vitis vinifera sp. Riesling on the formation of TDN, vitispiranes, and other volatile compounds[J]. Journal of Agricultural and Food Chemistry, 2020, 68(12): 3834−3849., articleTitle=null, refAbstract=null), Reference(id=1320881004798132982, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=32, rfOrder=31, authorNames=null, journalName=null, refType=null, unstructuredReference=MUÑOZ-REDONDO J M, RUIZ-MORENO M J, PUERTAS B, et al. Multivariate optimization of headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry for the analysis of terpenoids in sparkling wines[J]. Talanta, 2020, 208: 120483., articleTitle=null, refAbstract=null), Reference(id=1320881004886213367, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=33, rfOrder=32, authorNames=null, journalName=null, refType=null, unstructuredReference=TARASOV A, GIULIANI N, DOBRYDNEV A, et al. Absorption of 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) from wine by bottle closures[J]. European Food Research and Technology, 2019, 245(11): 2343−2351., articleTitle=null, refAbstract=null), Reference(id=1320881004949127928, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=34, rfOrder=33, authorNames=null, journalName=null, refType=null, unstructuredReference=PISANIELLO L, WATSON F, SIEBERT T, et al. The varietal influence of flavour precursors from grape Marc on monoterpene and C13-norisoprenoid profiles in wine as determined by membrane-assisted solvent extraction (MASE) GC-MS[J]. Molecules, 2022, 27(7): 2046., articleTitle=null, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1320880994702443163, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, xref=null, ext=[AuthorCompanyExt(id=1320880994710831772, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, companyId=1320880994702443163, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=State Key Laboratory of High-Efficiency Utilization of Coal and Green Chemical Engineering, College of Chemistry and Chemical Engineering, Ningxia University, Yinchuan 750021, China), AuthorCompanyExt(id=1320880994719220381, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, companyId=1320880994702443163, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=宁夏大学化学化工学院，省部共建煤炭高效利用与绿色化工国家重点实验室，宁夏银川 750021)])], figs=[ArticleFig(id=1320880998854804158, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.1, caption=Schematic diagram of the MSPE method, figureFileSmall=ndFSOIq+wogF2laCo6APFg==, figureFileBig=sKlbjiZihaGEZGBwXN4SZQ==, tableContent=null), ArticleFig(id=1320880998917718719, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图1, caption=MSPE方法示意图, figureFileSmall=ndFSOIq+wogF2laCo6APFg==, figureFileBig=sKlbjiZihaGEZGBwXN4SZQ==, tableContent=null), ArticleFig(id=1320880999022576320, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.2, caption=SEM images of materials, figureFileSmall=rO1q8ZBl0ktX8yHxB69nKg==, figureFileBig=4Sd7yZCYz8j98hX2JrOpoA==, tableContent=null), ArticleFig(id=1320880999089685185, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图2, caption=材料SEM图

注：（a）MNPs；（b）EG；（c）MEG；（d）MEG的元素映射图。

, figureFileSmall=rO1q8ZBl0ktX8yHxB69nKg==, figureFileBig=4Sd7yZCYz8j98hX2JrOpoA==, tableContent=null), ArticleFig(id=1320880999165182658, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.3, caption=FT-IR spectra of EG, Fe3O4 and MEG, figureFileSmall=b63e4FIUnpyik+/I4z6IJA==, figureFileBig=WR8ZD8YmijAatRn34kmlgA==, tableContent=null), ArticleFig(id=1320880999249068739, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图3, caption=EG、Fe3O4和MEG的FT-IR谱图, figureFileSmall=b63e4FIUnpyik+/I4z6IJA==, figureFileBig=WR8ZD8YmijAatRn34kmlgA==, tableContent=null), ArticleFig(id=1320880999337149124, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.4, caption=Magnetisation curves of MEG and Fe3O4, figureFileSmall=5uZzdmeG+sHr5iHN1a/fUQ==, figureFileBig=pveYW5xceAiAP8NiNL/X8g==, tableContent=null), ArticleFig(id=1320880999408452293, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图4, caption=MEG和Fe3O4的磁化曲线

注：饱和磁化强度由VSM磁化曲线在高场强下的坪值直接读取。

, figureFileSmall=5uZzdmeG+sHr5iHN1a/fUQ==, figureFileBig=pveYW5xceAiAP8NiNL/X8g==, tableContent=null), ArticleFig(id=1320880999471366854, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.5, caption=N2 adsorption-desorption isotherms (a) and pore size distribution curves (b) for MEG and EG, figureFileSmall=14cBCyYmkOL3I7sYgnshpA==, figureFileBig=9CCC/3bI2F+YU5g1gc2blQ==, tableContent=null), ArticleFig(id=1320880999546864327, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图5, caption=MEG和EG的N2吸附-脱附等温线（a）和孔径分布曲线（b）, figureFileSmall=14cBCyYmkOL3I7sYgnshpA==, figureFileBig=9CCC/3bI2F+YU5g1gc2blQ==, tableContent=null), ArticleFig(id=1320880999639139016, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.6, caption=MSPE condition optimization, figureFileSmall=VAY4B6Up880uBQkeF7WJ9Q==, figureFileBig=K8TEPFPdcEJE3W1Z+bRM9g==, tableContent=null), ArticleFig(id=1320880999714636489, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图6, caption=MSPE条件的优化

注：（a）EG用量；（b）盐浓度；（c）萃取时间；（d）解吸剂种类；（e）解吸溶剂体积；（f）解吸时间；不同小写字母表示不同水平处理组之间差异显著（P<0.05）。

, figureFileSmall=VAY4B6Up880uBQkeF7WJ9Q==, figureFileBig=K8TEPFPdcEJE3W1Z+bRM9g==, tableContent=null), ArticleFig(id=1320880999781745354, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.7, caption=Chromatogram of GC-MS, figureFileSmall=gyyBSaqkHhRRJcnyxWk/KA==, figureFileBig=/FUOn96CUcO2PxyHvcgZuA==, tableContent=null), ArticleFig(id=1320880999832077003, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图7, caption=GC-MS色谱图

注：（a）TDN标准溶液（50 ng/mL），（b）加标（50 ng/mL）葡萄酒样品经过MSPE萃取后。

, figureFileSmall=gyyBSaqkHhRRJcnyxWk/KA==, figureFileBig=/FUOn96CUcO2PxyHvcgZuA==, tableContent=null), ArticleFig(id=1320880999899185868, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Fig.8, caption=IRI isosurfaces (a) and RDG scatter plot (b) of EG with TDN, standard coloring method and chemical explanation of sign (λ2)ρ on IRI isosurfaces (c), figureFileSmall=v4jxpGyQVrbmOgWXoib/9Q==, figureFileBig=7IwuVByYDRhrbwTQUpMlFA==, tableContent=null), ArticleFig(id=1320880999983071949, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=图8, caption=EG与TDN的IRI等值面（a）、RDG散点图（b）和IRI等值面上标准着色方法及sign（λ2）ρ的化学解释（c）, figureFileSmall=v4jxpGyQVrbmOgWXoib/9Q==, figureFileBig=7IwuVByYDRhrbwTQUpMlFA==, tableContent=null), ArticleFig(id=1320881000045986510, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Table 1, caption=

Retention time, qualitative/quantitative ions, and chemical structure of target compounds

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物保留时间（min）定量*/定性离子（m/z）化学结构
TDN16.05157*、142、172
二丙酮醇（I.S）11.0643*、58、59
), ArticleFig(id=1320881000117289679, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=表1, caption=

目标化合物的保留时间、定性/定量离子及化学结构

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物保留时间（min）定量*/定性离子（m/z）化学结构
TDN16.05157*、142、172
二丙酮醇（I.S）11.0643*、58、59
), ArticleFig(id=1320881000180204240, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Table 2, caption=

Analysis of the reproducibility and accuracy of the method

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物回收率±RSD（%，n=3）日内精密度（RSD%，n=5）日间精密度（RSD%，n=3）
0.05 ng/mL50 ng/mL100 ng/mL0.05 ng/mL50 ng/mL100 ng/mL0.05 ng/mL50 ng/mL100 ng/mL
TDN90.6±5.786.2±5.0103.0±5.43.84.15.26.75.98.8
), ArticleFig(id=1320881000243118801, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=表2, caption=

方法的重现性、准确性考察分析

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物回收率±RSD（%，n=3）日内精密度（RSD%，n=5）日间精密度（RSD%，n=3）
0.05 ng/mL50 ng/mL100 ng/mL0.05 ng/mL50 ng/mL100 ng/mL0.05 ng/mL50 ng/mL100 ng/mL
TDN90.6±5.786.2±5.0103.0±5.43.84.15.26.75.98.8
), ArticleFig(id=1320881000327004882, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Table 3, caption=

Comparison of the MSPE method and other sample pretreatment methods for determining TDN in wine samples

, figureFileSmall=null, figureFileBig=null, tableContent=
样品前处理技术样品基质吸附剂材料前处理用时（min）仪器分析方法MDL（ng/mL）参考文献
HS-SPME雷司令葡萄酒PDMSa>30GC-MS0.01[31
HS-SPME起泡葡萄酒DVB/CAR/PDMSb69GC-MS0.08[32]
SBSE白葡萄酒PDMS>60GC-MS0.01[33]
MASE白葡萄酒正己烷/丙酮60GC-MS0.03[34]
MSPE雷司令葡萄酒MEG5cGC-MS0.01本研究
), ArticleFig(id=1320881000410890963, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=表3, caption=

MSPE新方法与其他样品前处理方法在测定葡萄酒样品中TDN的比较

, figureFileSmall=null, figureFileBig=null, tableContent=
样品前处理技术样品基质吸附剂材料前处理用时（min）仪器分析方法MDL（ng/mL）参考文献
HS-SPME雷司令葡萄酒PDMSa>30GC-MS0.01[31
HS-SPME起泡葡萄酒DVB/CAR/PDMSb69GC-MS0.08[32]
SBSE白葡萄酒PDMS>60GC-MS0.01[33]
MASE白葡萄酒正己烷/丙酮60GC-MS0.03[34]
MSPE雷司令葡萄酒MEG5cGC-MS0.01本研究
), ArticleFig(id=1320881000482194132, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=EN, label=Table 4, caption=

Native detected concentrations of TDN and recoveries with relative standard deviations at different spiking levels in three Riesling wine samples (n=3)

, figureFileSmall=null, figureFileBig=null, tableContent=
样品基质化合物检出浓度
（ng/mL）		回收率±RSD（%，n=3）
0.0550100
甜型雷司令葡萄酒TDN5.0（6.9）99.0±8.383.7±5.985.8±4.7
干型雷司令葡萄酒TDN14.2（1.7）85.1±2.683.4±2.284.4±3.4
半干型雷司令葡萄酒TDN9.1（1.6）91.4±8.281.3±3.685.2±5.1
), ArticleFig(id=1320881000549302997, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320880758223389403, language=CN, label=表4, caption=

三种雷司令葡萄酒样品中TDN的本底检出浓度及不同加标水平下的回收率和相对标准偏差（n=3）

, figureFileSmall=null, figureFileBig=null, tableContent=
样品基质化合物检出浓度
（ng/mL）		回收率±RSD（%，n=3）
0.0550100
甜型雷司令葡萄酒TDN5.0（6.9）99.0±8.383.7±5.985.8±4.7
干型雷司令葡萄酒TDN14.2（1.7）85.1±2.683.4±2.284.4±3.4
半干型雷司令葡萄酒TDN9.1（1.6）91.4±8.281.3±3.685.2±5.1
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高慧慧 , 靳候鑫 , 白红存 , 郑浩博 *
食品工业科技 | 分析检测 2026,47(17): 368-376
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磁固相萃取-气相色谱-质谱联用法高效分析葡萄酒中1,1,6-三甲基-1,2-二氢萘
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高慧慧 , 靳候鑫, 白红存, 郑浩博*
作者信息
  • 宁夏大学化学化工学院，省部共建煤炭高效利用与绿色化工国家重点实验室，宁夏银川 750021
通讯作者:
郑浩博（1989−），男，博士，副教授，研究方向：分离科学与技术，E-mail：。
作者简介:

高慧慧（1997−），女，硕士研究生，研究方向：分离科学与技术，E-mail：

Magnetic Solid-phase Extraction Coupled with Gas Chromatography-Mass Spectrometry for Efficient Analysis of 1,1,6-Trimethyl-1,2-dihydronaphthalene in Wine
Huihui GAO , Houxin JIN, Hongcun BAI, Haobo ZHENG*
Affiliations
  • State Key Laboratory of High-Efficiency Utilization of Coal and Green Chemical Engineering, College of Chemistry and Chemical Engineering, Ningxia University, Yinchuan 750021, China
出版时间: 2026-09-01 doi: 10.13386/j.issn1002-0306.2025080033
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摘要
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为解决雷司令葡萄酒中痕量特征香气物质1,1,6-三甲基-1,2-二氢萘（1,1,6-trimethyl-1,2-dihydronaphthalene，TDN）精准测定难题，本研究旨在建立一种基于磁性膨胀石墨（magnetic expanded graphite，MEG）的高效磁固相萃取-气相色谱-质谱联用分析新方法，通过简便的物理共混法制备MEG吸附剂，系统表征其理化性质，并优化了MSPE前处理的关键参数。同时，采用密度泛函理论计算从分子层面探究了吸附机理。结果表明，该方法在0.05~100 ng/mL范围内线性关系良好（R2=0.9943），检出限低至0.01 ng/mL。理论计算证实，范德华力与π–π堆积的协同作用（结合能−0.84 eV）是实现TDN高效吸附的关键驱动力。该方法已成功应用于多种雷司令葡萄酒样品，展现出目标化合物定量分析的高效性、准确性和可靠性。本研究不仅建立了一种快速、灵敏的TDN分析工具，也为基于理论计算指导新型食品风味物质富集材料的设计与应用提供了新思路。

1,1,6-三甲基-1,2-二氢萘（TDN）  /  磁固相萃取（MSPE）  /  气相色谱-质谱法（GC-MS）  /  雷司令葡萄酒  /  密度泛函理论（DFT）  /  风味分析

This study aimed to establish a novel and efficient analytical method based on magnetic expanded graphite (MEG) solid-phase extraction coupled with gas chromatography-mass spectrometry to address the challenge of accurately determining the trace characteristics of the aroma compound 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) in Riesling wines. The MEG adsorbent was prepared via a facile physical blending method, and its physicochemical properties were systematically characterized. Additionally, the key parameters affecting the magnetic solid-phase extraction (MSPE) pretreatment were optimized. Furthermore, density functional theory calculations were employed to investigate the adsorption mechanism at the molecular level. The results indicated that the method exhibited good linearity in the range of 0.05~100 ng/mL (R2=0.9943), with a limit of detection as low as 0.01 ng/mL. Theoretical calculations confirmed that the synergistic effect of van der Waals forces and π–π stacking (binding energy: −0.84 eV) was the key driving force for the efficient adsorption of TDN. The proposed method was successfully applied to the analysis of various Riesling wine samples, demonstrating high efficiency, accuracy, and reliability in the quantitative analysis of the target compound. This study not only provides a rapid and sensitive analytical tool for TDN but also offers new insights guided by theoretical calculations for the design and application of novel enrichment materials for food flavor compounds.

1,1,6-trimethyl-1,2-dihydronaphthalene (TDN)  /  magnetic solid-phase extraction (MSPE)  /  gas chromatography-mass spectrometry (GC-MS)  /  riesling wine  /  density functional theory (DFT)  /  flavor analysis
高慧慧, 靳候鑫, 白红存, 郑浩博. 磁固相萃取-气相色谱-质谱联用法高效分析葡萄酒中1,1,6-三甲基-1,2-二氢萘. 食品工业科技, 2026 , 47 (17) : 368 -376 . DOI: 10.13386/j.issn1002-0306.2025080033
Huihui GAO, Houxin JIN, Hongcun BAI, Haobo ZHENG. Magnetic Solid-phase Extraction Coupled with Gas Chromatography-Mass Spectrometry for Efficient Analysis of 1,1,6-Trimethyl-1,2-dihydronaphthalene in Wine[J]. Science and Technology of Food Industry, 2026 , 47 (17) : 368 -376 . DOI: 10.13386/j.issn1002-0306.2025080033
正文
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葡萄酒挥发性香气成分是决定其感官品质的重要因素[1]。在雷司令葡萄酒中，C13-降异戊二烯衍生物1,1,6-三甲基-1,2-二氢萘（1,1,6-trimethyl-1,2-dihydronaphthalene，TDN）是一种重要的品种特征香气化合物[2]。TDN以其标志性的煤油/石油气味在感官评价中发挥着关键作用[3]：在低浓度（<20 μg/L）下，TDN被认为是雷司令葡萄酒陈年香气复杂性与品种典型性的理想成分[4]；在较高浓度（>30 μg/L）下，其风味贡献转为负面，强烈掩盖了果香，成为品质缺陷[5]。因此，开发一种能够精准定量TDN的方法，对于客观评价雷司令葡萄酒的香气品质、指导酿造工艺以及优化贮藏条件具有重要意义[6]。然而，葡萄酒的样品基质复杂，TDN的含量相对较低，在使用仪器定量分析前必须采用高效的样品前处理方法对其进行有效的分离/富集。目前，分离/富集TDN的主流样品前处理技术为固相微萃取（solid-phase microextraction，SPME）技术[7]。尽管SPME有着灵敏度高、测定准确、使用溶剂量少等优点[8]。但该技术也存在自身局限性，如萃取纤维本身萃取相体积较小导致萃取能力有限[9]，且萃取动力学缓慢，限制了该技术的高效、快速分析。
为克服上述局限性，本研究提出一种基于磁固相萃取（magnetic solid-phase extraction，MSPE）的新型葡萄酒样品前处理策略。MSPE作为分散固相萃取的重要分支，通过将磁性吸附剂直接分散于样品中，极大地提升了传质效率[10]，并可利用外加磁场实现快速的固液分离[11]，兼具操作简便、快速高效、绿色环保的优点[12]。开发新型MSPE方法的关键在于设计对目标化合物具有高亲和力的磁性吸附剂[13]。膨胀石墨（expanded graphite，EG）作为一种三维多孔碳材料，其富含离域π电子的疏水表面[14]，可通过π-π堆积及疏水相互作用高效捕获具有芳环结构的TDN分子，是实现选择性吸附的理想材料[15]。基于此，本研究采用简便的物理共混法将Fe3O4纳米颗粒与EG复合，成功制备了兼具高效吸附性能与快速磁响应性的磁性膨胀石墨（magnetic expanded graphite，MEG）吸附剂。其创新之处在于，将EG对TDN的高亲和力同磁固相萃取的快速分离优势相结合，突破了传统SPME技术在分析葡萄酒中痕量TDN时存在的萃取容量低、动力学缓慢等瓶颈。
因此，本研究旨在开发一种基于MEG吸附剂的磁固相萃取-气相色谱-质谱联用（magnetic solid-phase extraction-gas chromatography-mass spectrometry，MSPE-GC-MS）新方法，用于雷司令葡萄酒中痕量TDN的精准分析。这项工作包括建立并优化高效、可靠的分析方法学，克服传统技术在灵敏度和处理效率上的不足；结合实验与DFT计算，从分子层面阐明EG对TDN的关键吸附机理。研究有望为复杂基质中关键风味分子的选择性富集提供理论依据，并为碳基吸附材料的理性设计提供新思路。
1　材料与方法
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1.1　材料与仪器
雷司令葡萄酒　购自银川本地超市，包括半甜型、甜型、半干型和干型四种类型；膨胀石墨　纯度98.0%，100目，膨胀温度900 ℃，江苏先丰纳米材料科技有限公司；1,1,6-三甲基-1,2-二氢萘（TDN）标准品　纯度>95.0%，杭州辅润医药科技有限公司；二丙酮醇（内标化合物）　色谱纯，上海阿拉丁生化科技股份有限公司；氯化钠（NaCl）、乙二醇、乙酸钠、六水合三氯化铁（FeCl3·6H2O）　分析纯，上海麦克林有限公司；乙腈、环己烷、正己烷、丙酮、乙二胺　色谱纯，国药集团化学试剂有限公司。
GCMS-QP2020NX气相色谱-质谱联用仪　配置自动进样模块AOC-20i+s，日本岛津公司；ZEISS Sigma 300扫描电子显微镜（Scanning electron microscopy，SEM）　德国卡尔·蔡司股份公司；Nicolet iS5型傅里叶变换红外（Fourier transform infrared，FT-IR）光谱仪　美国赛默飞世尔科技有限公司；Lake Shore 8604型振动样品磁强计（Vibrating Sample Magnetometer，VSM）　美国Lake Shore公司；Micromeritics ASAP 2460型比表面积和孔径分析仪　美国麦克仪器公司。
1.2　实验方法
1.2.1　MEG的制备
本研究采用溶剂热法合成Fe3O4纳米颗粒[16]。具体步骤如下：称取 20.0 g FeCl3·6H2O溶解于400 mL乙二醇中，随后缓慢加入60.0 g乙酸钠及200 mL乙二胺。将所得混合溶液磁力搅拌30 min，直至溶液澄清。随后将该溶液转移至1 L聚四氟乙烯内胆中，密封后置于不锈钢高压反应釜内，200 ℃下反应 8 h。反应结束后，自然冷却至室温，利用外加磁场分离产物，并用蒸馏水和无水乙醇交替超声清洗数次。最后，将所得黑色产物（Fe3O4）置于真空干燥箱中，60 ℃干燥12 h备用。
MEG磁性吸附剂通过物理共混法制备。准确称取20 mg Fe3O4纳米颗粒与5 mg EG置于研钵中，充分研磨混匀，即得MEG复合材料。
1.2.2　材料表征
1.2.2.1　扫描电子显微镜
采用扫描电子显微镜观察材料的微观形貌。材料的元素组成与分布通过该设备搭载的能量色散X射线光谱（energy dispersive spectrometer，EDS）分析仪进行测定。
1.2.2.2　傅里叶变换红外（FT-IR）光谱
通过傅里叶变换红外光谱仪分析材料表面的化学官能团。将样品与溴化钾按质量比 1:100 混合、研磨均匀后，压制成半透明的薄片进行测试。光谱扫描范围为4000~400 cm−1。
1.2.2.3　磁化曲线
使用振动样品磁强计在室温下测量材料的磁化曲线。将适量粉末样品装入样品管中固定，在±20 kOe的外加磁场范围内进行磁化强度的测定。
1.2.2.4　N2吸附-脱附等温线和孔径分布
材料的比表面积及孔径分布通过全自动比表面积与孔隙度分析仪进行N2吸附-脱附等温线测试。测试前，所有样品均在120 ℃的温度下真空脱气6 h。在77 K的液氮温度下进行测试。比表面积由Brunauer-Emmett-Teller（BET）模型在相对压力（P/P0）为0.05~0.3的范围内计算得出。孔径分布则由Barrett-Joyner-Halenda（BJH）模型从脱附支等温线数据计算得到。
1.2.3　MSPE法萃取葡萄酒中TDN
使用色谱纯丙酮作为溶剂，将TDN和二丙酮醇（内标，I.S.）标准品分别配制为浓度1.0 mg/mL的储备溶液。后续实验中，将储备溶液进一步稀释至10 mg/L，以此作为工作溶液。上述标准溶液均在4 ℃冰箱中避光保存。
在5 mL葡萄酒样品中加入二丙酮醇内标工作溶液至浓度为10 ng/mL，静置一段时间后，加入5 mL蒸馏水稀释，随后在10 mL稀释葡萄酒样品中加入氯化钠至盐浓度为200 mg/mL，备用。
本研究设计的MSPE方法步骤如下。如图1所示，称取25 mg MEG吸附剂于15 mL玻璃瓶中，再加入10 mL经上述处理的葡萄酒样品，强烈振荡2 min进行萃取，吸附了TDN的MEG在外加磁场下与样品溶液分离，弃去上清液。随后加入100 μL乙腈，强烈振荡3 min来解吸MEG上的TDN。最终在外加磁场下实现固液分离，收集澄清的解吸液进行GC-MS分析，无需过滤操作。
1.2.4　GC-MS条件
色谱柱：SH-Stabilwax-DA 30 m （length）×0.25 mm （i.d.）×0.25 μm；升温程序参考Sacks等[17]并有所改动：柱温箱的初始温度设置为40 ℃，保持3.0 min；然后以10 ℃/min的速率升温至170 ℃，保持2.0 min，再以20 ℃/min的速率升温至230 ℃并保持5 min；在不分流条件下进样1.0 μL；载气为纯度≥99.999%的高纯氦气，流速为1.0 mL/min；进样口温度为230 ℃，离子源温度为200 ℃，接口温度为230 ℃；使用电子轰击离子源；电子能量70 eV；目标化合物的定性离子与定量离子的相关信息见表1。
定性方法：依据色谱保留时间与质谱特征碎片离子信息进行双重鉴别。在相同仪器分析条件下，样品中待测化合物的色谱峰的保留时间应与TDN标准品一致；在选择离子监测模式下，该待测化合物的特征离子（m/z 157、142、172）相对丰度与TDN标准品的偏差应小于30%。
定量方法：采用以内标校正的标准曲线法对TDN进行定量分析。其方程如式（1）：
$\rm Y=aX+b $
式中，Y为TDN与内标物的峰面积比，X为样品浓度（ng/mL），a，b分别为标准曲线的斜率和截距。
实际样品中TDN的浓度（Cx）计算公式如式（2）：
$\rm Cx(ng/mL)=\frac{(Yx-b)}{a} $
式中，Cx为实际样品中TDN的测定浓度（ng/mL），Yx为TDN与内标物峰面积比，a，b分别为标准曲线的斜率和截距。
1.2.5　MSPE条件的优化
为获得最佳的样品前处理效果，本研究采用单因素序贯优化策略，在TDN加标（50 ng/mL）的葡萄酒样品基质中，对MSPE关键参数进行了系统考察。固定吸附剂中Fe3O4纳米颗粒用量为20 mg，其余各初始条件如下：EG 5 mg，盐（NaCl）浓度200 mg/mL，萃取时间2 min，解吸溶剂100 μL乙腈，解吸时间3 min。在确定某一参数的最佳值后，将其取代初始参数，用于后续其他参数的优化。参数考察范围：EG用量（0、5、10、15、20 mg）、盐浓度（0、50、100、150、200、250 mg/mL）、萃取时间（0.5、1、2、3、4 min）、解吸剂种类（乙腈、正己烷、环己烷、丙酮）、解吸剂体积（100、150、200、250、300 μL）及解吸时间（0.5、1、2、3、4 min）。
在样品前处理条件优化阶段，为精确评估各MSPE条件对实验结果的影响，内标二丙酮醇于解吸步骤后加入解吸液中（终浓度100 ng/mL），其作用为校正仪器分析误差。所有优化实验均以TDN与内标峰面积比作为因变量，平行测定三次。
1.2.6　吸附机理
为了从分子层面深入探究MEG对TDN的吸附机理，本研究采用DFT进行计算。鉴于在MEG复合材料中，EG是提供吸附位点的主要功能组分，而Fe3O4纳米颗粒仅赋予其磁分离性能，因此计算模型简化为EG与TDN分子之间的相互作用。
本研究使用Gaussian 16构建了以单层石墨片层结构作为EG的简化模型，其结构仅由碳原子构成。随后，将TDN分子与EG模型置于相互作用的初始位置，并在B3LYP/6-31G （d）水平下对初始结构进行结构优化，得到最终的模型结构。
基于上述几何优化得到的稳定构象，通过Multiwfn 3.8程序[18]对相应的波函数计算结果进行后处理分析，并借助分子动力学可视化（Visual Molecular Dynamics，VMD）软件实现相互作用的可视化[19]。首先，通过计算结合能（ΔE）来定量评估两模型间的稳定性。其次，采用相互作用区域指示函数（interaction region indicator，IRI）[20]和约化密度梯度（reduced density gradient，RDG）来对EG与TDN之间的相互作用类型进行定性分析。
此外，根据式（3）计算EG与TDN之间的结合能ΔE。
$\rm \Delta E={E}_{AB}-{E}_{A}-{E}_{B}+{E}_{BSSE} $
式中：ΔE为结合能，EAB是EG与TDN之间相互作用的总能量，EA是EG模型的能量，EB是TDN的能量，EBSSE是基组重叠误差校正能（以上能量单位均为eV）；其中结合能越负，表明EG对TDN的吸附越强。
1.2.7　方法学考察
为全面评价新建立的MSPE-GC-MS方法的分析性能，本研究在最优化的前处理条件下，对方法的线性关系、灵敏度、精密度及准确度进行了系统考察。
本研究以半甜型雷司令葡萄酒作为样品基质，添加不同量的TDN标准溶液至浓度为0.05~100 ng/mL，将内标化合物浓度固定为10 ng/mL，以得到的平均峰面积比值对样品浓度进行线性回归，得到线性回归方程及决定系数（R2）。以信噪比（S/N）的3倍和10倍分别计算TDN的方法检出限（method detection limit，MDL）和方法定量限（method quantification limit，MQL）。
方法的重现性和准确性通过考察日内/日间精密度以及加标回收率来评估。本研究在半甜型雷司令葡萄酒样品中分别添加低（0.05 ng/mL）、中（50 ng/mL），高（100 ng/mL）三个浓度的TDN，用获得的实验数据计算相对标准偏差。在上述浓度下，以1 d内进行的五组平行实验的结果计算得出日内精密度；以连续3 d分别进行的独立重复实验结果计算得出日间精密度。精密度最终以相对标准偏差（RSD, %）表示，方法的准确度以加标回收率（%）表示。
1.2.8　实际雷司令葡萄酒样品中的应用
为验证新建立分析方法的适用性，本研究选取了三种不同类型的雷司令葡萄酒（甜型、干型、半干型）作为分析对象。首先，测定了各样品中TDN的本底浓度；随后，在低（0.05 ng/mL）、中（50 ng/mL）和高（100 ng/mL）三个浓度水平上进行了加标回收测试。所有样品分析均平行进行三次。
1.3　数据处理
除特殊说明外，所有数据均表示为3次重复实验的平均值±标准差，并使用IBM SPSS Statistics 26软件对数据进行单因素方差分析（ANOVA）和Duncan检验（P<0.05），并使用Origin 2022软件绘图。
为从理论层面揭示EG与TDN之间的相互作用机制，本研究采用DFT进行计算。所有计算均在Gaussian 16软件包[21]中完成，基于优化后的结构，利用Multiwfn 3.8程序进行波函数分析，并结合VMD软件进行可视化，最终生成IRI等值面和RDG散点图，用于定性识别和分析分子间的相互作用力。
2　结果与分析
收起
2.1　EG与MEG的材料表征
利用扫描电子显微镜对Fe3O4、EG和MEG的微观形貌进行了表征（图2a~图2c）。结果显示Fe3O4呈球状，粒径均一，尺寸在50 nm左右（图2a）；膨胀石墨呈现出不规则的多片层结构，与文献报道一致[14]（图2b）；MEG的SEM图（图2c）可观察到Fe3O4嵌入膨胀石墨片层之间或附着在片层结构上，表明Fe3O4与EG成功复合。元素映射分析（图2d）进一步证实了C、O、Fe三种元素在复合材料中的均匀分布，有力地证明了MEG的成功制备。
根据本课题组前期用物理共混法制备的磁性吸附剂的研究[22]，可以推断MEG的形成是源于“团聚机理”。Fe3O4在许多溶剂中有团聚趋势，因此当EG同Fe3O4均匀混合并在溶剂中分散，Fe3O4有可能通过团聚附着于EG上，从而生成MEG。MEG的SEM图也可佐证这一猜测。
材料的化学结构通过傅里叶变换红外（FT-IR）光谱进一步确认（图3）。3413 cm−1处的宽吸收峰归属于O-H键伸缩振动[23]，这可能源于水分子的红外吸收；1622 cm−1处出现的峰对应于膨胀石墨骨架中芳环的C=C键的伸缩振动[24]；从图中可明显看出EG与MEG的特征峰基本相对应，进一步说明物理共混法对EG的化学结构没有明显影响，可最大程度地保留其吸附位点。与纯EG的图谱相比，MEG在599 cm−1处出现了一个新的、显著的吸收峰，该峰归属于Fe-O键的伸缩振动[23]，再次证实了Fe3O4与EG的成功复合。
图4给出了室温下MEG与Fe3O4的磁化曲线，可以明显看到，两种材料的磁化曲线均未呈现磁滞回线，表明材料为超顺磁性。且MEG的饱和磁化强度为52.5 emu/g，可保证在20 s内实现磁分离。
材料的孔隙结构通过N2吸附-脱附等温线进行了分析（图5a）。根据IUPAC分类，EG和MEG均表现出典型的IV型等温线，表明两者均富含介孔结构。其中，EG呈现H4型回滞环，这与膨胀石墨片层堆积形成的裂缝状孔隙特征相符；而MEG则呈现H1型回滞环，表明Fe3O4纳米颗粒的复合使得材料形成了更为规整、均一的介孔。其BET比表面积也从17.73 m2/g增加至37.26 m2/g。从孔径分布图（图5b）可以看出，与EG相比，MEG在微孔区域（<2 nm）出现了新的孔径分布，证明复合过程中不仅增大了比表面积，还形成了微孔-介孔共存的多级孔道结构，非常有利于吸附过程。
2.2　MSPE条件的优化
2.2.1　吸附剂的用量
吸附剂的用量是影响萃取效率的关键因素。本研究首先通过实验确定了Fe3O4:EG=1:1 （w/w）时，足以实现吸附剂的快速磁分离，且Fe3O4自身对TDN几乎没有吸附能力（图6a，EG用量为0 mg时）。因此，本研究固定Fe3O4用量为20 mg，考察EG用量（0~20 mg）对萃取效率的影响。如图6a所示，随着EG用量从0 mg增加至5 mg，TDN的萃取效率显著提高（P<0.05）；然而，当EG用量进一步增加至20 mg时，峰面积比呈现轻微下降趋势。该现象可从吸附和解吸两方面解释：一方面，吸附剂过少会直接导致TDN萃取不完全，因此得到较低的峰面积比；另一方面，在解吸剂体积固定为100 μL的前提下，过量的吸附剂（>5 mg）虽然可能吸附更多的TDN，但有限的解吸试剂不足以将目标化合物从吸附剂表面完全洗脱下来，从而导致解吸效率的降低[16]。因此，将EG用量固定为5 mg。
2.2.2　盐浓度
本研究通过增加NaCl浓度（0~250 mg/mL），来考察盐浓度对MEG萃取效率的影响。如图6b所示，当盐浓度从0 mg/mL增加至200 mg/mL时，TDN的峰面积显著提升（P<0.05）；继续增大盐浓度，峰面积比趋于稳定。这归因于盐析效应：高离子强度降低了TDN在葡萄酒样品中的溶解度，使其更容易因疏水作用被MEG所吸附[25]。因此，选择200 mg/mL 盐浓度进行后续实验。
2.2.3　萃取时间
本研究将萃取时间从0.5 min增加至4 min，以考察其对萃取效率的影响。如图6c所示，随着萃取时间从0.5 min增加至2 min，萃取效率明显提高；继续延长萃取时间，峰面积比没有明显变化，表明在2 min时，TDN在吸附剂与样品基质之间已达到分配平衡[23]。因此，确定最佳萃取时间为2 min。
2.2.4　解吸条件
解吸剂的类型直接影响解吸效率。本研究考察了常见的四种有机溶剂：环己烷、正己烷、丙酮和乙腈。如图6d所示，乙腈表现出高于其他溶剂的解吸效率。造成该现象的原因可能是乙腈分子的氰基（-C≡N）能作为有效的π电子作用位点，与膨胀石墨表面发生强烈的竞争性π-π相互作用，从而将TDN分子从吸附位点上有效置换下来[26]。因此，本研究选用乙腈作为优化后的解吸试剂。
考察了解吸剂体积对解吸效率的影响。如图6e所示，随着乙腈用量增加，目标化合物在乙腈中的浓度由于稀释效应而降低[27]。然而，进一步减小解吸剂体积会导致操作不便。因此，最终选择100 μL乙腈作为最优解吸体积。
考察了解吸时间对解吸效率的影响。如图6f所示，3 min就足够将萃取的TDN从MEG表面解吸下来。因此，确定最佳解吸时间为3 min。
根据上述条件考察的结果，最终确定了该MSPE的最优条件：5 mg的EG用量；200 mg/mL的盐浓度；萃取时间为2 min；100 µL乙腈作为解吸剂；解吸时间为3 min。图7（b）为在最优条件下，从加标（50 ng/mL）葡萄酒样品中萃取出TDN并进入GC-MS检测的色谱图；图7（a）为TDN标准溶液的GC-MS色谱图（配制于丙酮，浓度为50 ng/mL）。从图中可明显看出，经过MSPE萃取后，TDN的信号强度明显增加，且无杂峰干扰，表明MEG可有效地从葡萄酒基质中分离/富集TDN。
2.3　潜在的吸附机理
为了深入探究EG与TDN之间的相互作用，本研究采用DFT进行计算，评估其潜在的吸附机制。首先，通过计算两者复合物的结合能（ΔE）来评估其结合的稳定性。计算结果显示，EG与TDN之间的结合能ΔE为−0.84 eV，表明EG能够在萃取过程中有效地吸附TDN。为了进一步揭示吸附本质，本研究生成了IRI等值面和RDG散点图。图8清晰展示了EG与TDN之间的相互作用区域。根据Lu等[28]的研究，IRI等值面图中的标准着色方法和sign（λ2）ρ的化学解释详见图8c，蓝色区域代表化学键、氢键等强相互作用，红色区域代表空间位阻效应，绿色区域代表范德华力、π-π相互作用等弱相互作用。在IRI等值面图（图8a）中，广泛分布且呈现扁平化的绿色区域表明，EG与TDN之间存在以色散力为主导的范德华力和π-π相互作用[29]。RDG散点图（图8b）提供了进一步的证据，图中在sign（λ2）ρ值约为−0.005 a.u.和0.005 a.u.处分别观察到明显的尖峰，这表明存在显著的范德华相互作用（分别对应吸引力和排斥力）[30]。这进一步证实了范德华力和π-π相互作用对吸附过程的主导作用。综上所述，DFT计算结合IRI和RDG分析共同表明，EG对TDN的吸附主要由范德华相互作用（以色散力为主）和π-π相互作用所驱动。这两种非共价作用力的协同效应是MEG材料能够高效富集葡萄酒中痕量TDN的关键原因。
2.4　方法学考察
为了评价本研究提出的方法的有效性，后续做了工作曲线、MDL、MQL、精密度及回收率等的相关实验和考察。
本研究以半甜型雷司令葡萄酒作为样品基质，添加不同量的TDN标准溶液至浓度为0.05~100 ng/mL，以得到的平均峰面积比值对样品浓度进行线性回归，得到线性回归方程及决定系数（R2）。实验结果表明：新方法在0.05~100 ng/mL的浓度范围内表现出良好的线性关系，拟合标准方程为Y=0.217X+0.0033，决定系数R2=0.9943。式中Y为目标化合物与内标物的信号强度（峰面积）比值，X为样品浓度。MDL和MQL分别低至0.01 ng/mL和0.03 ng/mL，低于TDN化合物的感官阈值，满足对葡萄酒中痕量TDN的检测需求。
方法的准确度与精密度通过在低（0.05 ng/mL）、中（50 ng/mL）、高（100 ng/mL）三个浓度水平的加标回收实验得到证实。方法的日内和日间精密度较高，RSD分别低于5.2%和8.8%；同时，在三个浓度水平下的平均加标回收率介于86.2%~103.0%（表2）。这些数据表明，本方法具有良好的准确度和精密度，能够满足复杂基质样品中痕量TDN的可靠定量分析要求。
为进一步评估本方法的应用价值，本研究将其与文献报道的主流技术进行了综合比较（表3）。结果显示，相较于业内广泛使用的顶空固相微萃取（headspace solid-phase microextraction，HS-SPME）技术及搅拌棒吸附萃取（stir bar sorptive extraction，SBSE）、膜辅助溶剂萃取（membrane-assisted solvent extraction，MASE）等样品前处理技术，本方法在确保同等甚至更高分析灵敏度的前提下，极大地缩短了样品前处理用时。这一对比结果清晰地表明，本研究为复杂基质中痕量TDN的快速、常规检测提供了一种具有竞争力的技术方案。
2.5　实际雷司令葡萄酒样品中的应用
为了验证新建立的MSPE-GC-MS方法的广泛适用性，本研究将该方法应用到甜型、干型、半干型三种雷司令葡萄酒样品中进行验证。对未加标样品的直接测定结果表明（表4），所有雷司令葡萄酒中均检出TDN，其浓度范围在5.0~14.2 ng/mL之间。加标回收实验结果进一步验证了本方法良好的准确性。如表4所示，在覆盖了整条工作曲线的低（0.05 ng/mL）、中（50 ng/mL）、高（100 ng/mL）三个浓度水平上，TDN在不同样品基质中加标回收率范围在81.3%~99.0%之间，且RSD皆低于8.3%。结果表明新方法可以满足多种雷司令葡萄酒中TDN分析的要求。
3　结论
收起
本研究成功建立了一种基于磁性膨胀石墨的磁固相萃取-气相色谱-质谱联用新方法，实现了雷司令葡萄酒中关键香气成分TDN的快速、灵敏测定。该方法展现出优异的分析性能：核心前处理步骤用时仅需5 min，显著提升了检测效率；方法灵敏度高，检出限低至0.01 ng/mL，并在0.05~100 ng/mL 范围内呈现良好的线性关系（R2=0.9943）；加标回收率为86.2%~103.0%，相对标准偏差（RSD）小于8.8%，证明了方法的高准确度与精密度。经DFT理论计算可知结合能为−0.84 eV，从分子层面揭示了吸附机理，证实范德华力与π-π堆积的协同作用是驱动MEG高效富集TDN的主导力量。综上所述，本研究不仅为葡萄酒品质控制提供了一种实用的分析工具，所展示的吸附剂设计与分析方法开发策略，也为复杂食品基质中其他关键风味物质的检测提供了有价值的参考。

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参考文献 引证文献
排序方式：
1
LI Na, LI Guanyu, GUAN Xuan, et al. Volatile aroma compound-based decoding and prediction of sweet berry aromas in dry red wine[J]. Food Chemistry, 2025, 463: 141248.
2
CAFFREY A J, LERNO L A, ZWEIGENBAUM J, et al. Characterization of free and bound monoterpene alcohols during Riesling fermentation[J]. Journal of Agricultural and Food Chemistry, 2021, 69(45): 13286−13298.
3
LI L Y. Memory1,1,6-trimethyl-1,2-dihydroxnapthalene (TDN) is a common odor defect of Riesling wine (petrol) that screams "Riesling" at subthreshold levels[D]. New York: Cornell University, 2025.
4
HAAG F, FREY T, BALL L, et al. Petrol note in Riesling-1,1, 6-trimethyl-1,2-dihydronaphthalene (TDN) selectively activates human odorant receptor OR8H1[J]. Journal of Agricultural and Food Chemistry, 2024, 72(9): 4888−4896.
5
ZIEGLER M, GÖK R, BECHTLOFF P, et al. Impact of matrix variables and expertise of panelists on sensory thresholds of 1,1,6-trimethyl-1,2-dihydronaphthalene known as petrol off-flavor compound in Riesling wines[J]. Food Quality and Preference, 2019, 78: 103735.
6
GÖK R, SELHORST P, KIENE M, et al. Target-guided isolation of progenitors of 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) from Riesling wine by high-performance countercurrent chromatography[J]. Molecules, 2022, 27(17): 5378.
7
ANTAL E, VARGA Z, KÁLLAY M, et al. 1,1,6-trimethyl-1,2-dihydronaphthalene content of Riesling wines in Hungary[J]. ACS Omega, 2023, 8(40): 36677−36685.
8
LESZCZYŃSKA D, HALLMANN A, TREDER N, et al. Recent advances in the use of SPME for drug analysis in clinical, toxicological, and forensic medicine studies[J]. Talanta, 2024, 270: 125613.
9
HAO Yaofei, LI Jianxun, ZHAO Zhiheng, et al. Flavor characteristics of Shanlan rice wines fermented for different time based on HS-SPME-GC-MS-O, HS-GC-IMS, and electronic sensory analyses[J]. Food Chemistry, 2024, 432: 137150.
10
CASTELL A, ARROYO-MANZANARES N, VIÑAS P, et al. Advanced materials for magnetic solid-phase extraction of mycotoxins: A review[J]. TrAC Trends in Analytical Chemistry, 2024, 178: 117826.
11
FU Quanbin, XIA Zhenzhen, SUN Xin, et al. Recent advance and applications of covalent organic frameworks based on magnetic solid-phase extraction technology for food safety analysis[J]. TrAC Trends in Analytical Chemistry, 2023, 162: 117054.
12
JAFARI Z, GHANI M. Magnetic carbonized cellulose-MIL 101(Fe) composite as a sorbent for magnetic solid phase extraction of selected organophosphorus pesticides combined with high performance liquid chromatography-ultraviolet detection[J]. Talanta Open, 2023, 7: 100212.
13
ZHAO Mingming, WU Haizhi, DENG Xiaoke, et al. The application progress of magnetic solid-phase extraction for heavy metal analysis in food: A mini review[J]. Analytical Methods, 2024, 16(3): 333−343.
14
ELBIDI M, MOHD SALLEH M A, RASHID S A, et al. The potential of thermally expanded graphite in oil sorption applications[J]. RSC Advances, 2024, 14(23): 16466−16485.
15
SUN Kangkang, LIU Muyu, SUN Kaige, et al. High-efficiently and rapidly capturing cesium from water with Prussian blue@expanded graphite as adsorbent[J]. Journal of Industrial and Engineering Chemistry, 2023, 125: 336−344.
16
ZHENG Haobo, DING Jun, ZHENG Shujian, et al. Facile synthesis of magnetic carbon nitride nanosheets and its application in magnetic solid phase extraction for polycyclic aromatic hydrocarbons in edible oil samples[J]. Talanta, 2016, 148: 46−53.
17
SACKS G L, GATES M J, FERRY F X, et al. Sensory threshold of 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) and concentrations in young Riesling and non-Riesling wines[J]. Journal of Agricultural and Food Chemistry, 2012, 60(12): 2998−3004.
18
LU Tian, CHEN Feiwu. Multiwfn: A multifunctional wavefunction analyzer[J]. Journal of Computational Chemistry, 2012, 33(5): 580−592.
19
HUMPHREY W, DALKE A, SCHULTEN K. VMD: Visual molecular dynamics[J]. Journal of Molecular Graphics, 1996, 14(1): 33−38.
20
JOHNSON E R, KEINAN S, MORI-SÁNCHEZ P, et al. Revealing noncovalent interactions[J]. Journal of the American Chemical Society, 2010, 132(18): 6498−6506.
21
FRISCH M, TRUCKS G, SCHLEGEL H, et al. St: Gaussian 16 revision C. 01[J]. Gaussian Inc, Wallingford CT, 2016.
22
ZHENG Haobo, DING Jun, ZHENG Shujian, et al. Magnetic "one-step" quick, easy, cheap, effective, rugged and safe method for the fast determination of pesticide residues in freshly squeezed juice[J]. Journal of Chromatography A, 2015, 1398: 1−10.
23
WANG Bin, CHEN Yongyue, LI Wenxuan, et al. Magnetic phytic acid-modified kapok fiber biochar as a novel sorbent for magnetic solid-phase extraction of antidepressants in biofluids[J]. Analytica Chimica Acta, 2024, 1296: 342295.
24
HOU Bo, SUN Hongjuan, PENG Tongjiang, et al. Rapid preparation of expanded graphite at low temperature[J]. New Carbon Materials, 2020, 35(3): 262−268.
25
ZHANG Kaige, WANG Jing, GUO Rong, et al. Acid induced dispersive liquid-liquid microextraction based on in situ formation of hydrophobic deep eutectic solvents for the extraction of bisphenol A and alkylphenols in water and beverage samples[J]. Food Chemistry, 2024, 442: 138425.
26
KARAPıNAR H S, BALıKÇıOĞLU A. Boron-doped activated carbon nanocomposite as a selective adsorbent for rapid extraction of aflatoxins in nut samples[J]. Journal of Food Composition and Analysis, 2022, 112: 104680.
27
LI Min, LIU Weihua, MENG Xufeng, et al. Facile synthesis of magnetic hypercrosslinked polymer for the magnetic solid-phase extraction of benzoylurea insecticides from honey and apple juice samples[J]. Food Chemistry, 2022, 395: 133596.
28
LU Tian, CHEN Qinxue. Interaction region indicator: A simple real space function clearly revealing both chemical bonds and weak interactions[J]. Chemistry-Methods, 2021, 1(5): 231−239.
29
FAN Sheng, LU Xinru, LI Haoliang, et al. Efficient removal of organophosphate esters by ligand functionalized MIL-101 (Fe): Modulated adsorption and DFT calculations[J]. Chemosphere, 2022, 302: 134881.
30
WANG Bin, XU Shuangjiao, LI Wenxuan, et al. Polyaniline-coated kapok fibers for convenient in-syringe solid-phase microextraction and determination of organochlorine and pyrethroid pesticide residues in aqueous samples[J]. Talanta, 2024, 271: 125706.
31
ZIEGLER M, WEGMANN-HERR P, SCHMARR H G, et al. Impact of rootstock, clonal selection, and berry size of Vitis vinifera sp. Riesling on the formation of TDN, vitispiranes, and other volatile compounds[J]. Journal of Agricultural and Food Chemistry, 2020, 68(12): 3834−3849.
32
MUÑOZ-REDONDO J M, RUIZ-MORENO M J, PUERTAS B, et al. Multivariate optimization of headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry for the analysis of terpenoids in sparkling wines[J]. Talanta, 2020, 208: 120483.
33
TARASOV A, GIULIANI N, DOBRYDNEV A, et al. Absorption of 1,1,6-trimethyl-1,2-dihydronaphthalene (TDN) from wine by bottle closures[J]. European Food Research and Technology, 2019, 245(11): 2343−2351.
34
PISANIELLO L, WATSON F, SIEBERT T, et al. The varietal influence of flavour precursors from grape Marc on monoterpene and C13-norisoprenoid profiles in wine as determined by membrane-assisted solvent extraction (MASE) GC-MS[J]. Molecules, 2022, 27(7): 2046.
2026年第47卷第17期
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doi: 10.13386/j.issn1002-0306.2025080033
  • 接收时间：2025-08-11
  • 首发时间：2026-10-24
  • 出版时间：2026-09-01
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  • 收稿日期：2025-08-11
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    宁夏大学化学化工学院，省部共建煤炭高效利用与绿色化工国家重点实验室，宁夏银川 750021

通讯作者:

郑浩博（1989−），男，博士，副教授，研究方向：分离科学与技术，E-mail：。
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2种不同金属材料的力学参数
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Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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