Article(id=1151437191097447023, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151437189243089177, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250226004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1740499200000, receivedDateStr=2025-02-26, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752453619025, onlineDateStr=2025-07-14, pubDate=1749916800000, pubDateStr=2025-06-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752453619025, onlineIssueDateStr=2025-07-14, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752453619025, creator=13701087609, updateTime=1752453619025, updator=13701087609, issue=Issue{id=1151437189243089177, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='11', pageStart='1', pageEnd='320', issueExtLink='null', onlineDate='null', pubDate='1749916800000', pubDateStr='2025-06-15', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752453618584, creator='13701087609', updateTime=1767768054466, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1215670588966883492, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151437189243089177, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1215670588966883493, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1151437189243089177, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=68, endPage=77, ext={EN=ArticleExt(id=1151895326140018699, articleId=1151437191097447023, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Analysis of flavor compounds in Douzhir and Ma Tofu based on purge and trap-gas chromatography/mass spectrometry, columnId=1151895321849721368, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Food Flavor Research, runingTitle=null, highlight=null, articleAbstract=

Objective To identify flavor compounds in Douzhir and Ma Tofu and analyze their characteristic components based on purge and trap-gas chromatography/mass spectrometry (PT-GC/MS) combined with the national institute of standards and technology (NIST) database. Methods Weigh 2.0 g of sample into a 40 mL brown spiral sample bottle, add 10 mL of experimental water and a tetrafluoroethylene magnetic stirrer, heat the sample at 40 ℃, and analyze it by PT-GC/MS. Results A total of 260 kinds of flavor compounds were identified across 34 batches, including sulfur-containing compounds, alcohols, aldehydes, ketones, esters, etc. Raw and cooked Douzhir exhibited significantly higher relative abundances of sulfur-containing compounds compared to Ma Tofu, which showed greater diversity but lower similarity in flavor profiles. These identification data could to some extent reflect sensory evaluation results, but there was a possibility that some flavor compounds might be more prominent or interfered with by other odors. In addition, this study used principal component analysis (PCA) method to identify the overall distribution of samples and deviations from samples, and attempted to analyze the reasons for deviations. Further, using orthogonal partial least squares discriminant analysis (OPLS-DA), based on the screening conditions [P<0.05, variable importance in the projection (VIP)>1], 31 kinds of characteristic flavor compounds of raw and cooked Douzhir were selected, which could be used for the differentiation and identification of raw and cooked Douzhir. Conclusion The study confirms that PT-GC/MS combined with multivariate statistical method can effectively analyze the flavor compounds of Douzhir and Ma Tofu, screen the characteristic compounds, and provide a basis for the subsequent optimization and improvement of product flavor.

, authors=null, authorsList=Zhi-Chao YANG, Ying LIANG, Hai-Xian JIA, Chun-Yu LI, Chun-Mei ZHANG, Qiao-Yun MA, Xiao-Chen MA, Yue-Chao FENG, Peng SHAO, Li-Li MA, authorCompany=null, correspAuthors=Li-Li MA, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, 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=1151895342174843354, articleId=1151437191097447023, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=基于吹扫捕集-气相色谱/质谱法分析豆汁、麻豆腐中风味物质, columnId=1151895322046853658, journalTitle=食品安全质量检测学报, columnName=本期专题:食品风味研究, runingTitle=null, highlight=null, articleAbstract=

目的 基于吹扫捕集-气相色谱/质谱法(purge and trap-gas chromatography/mass spectrometry, PT-GC/MS)并结合美国国家标准与技术研究院(national institute of standards and technology, NIST)数据库, 鉴定豆汁、麻豆腐中的风味物质并分析其特征物质。方法 称取2.0 g样品, 于40 mL棕色螺旋样品瓶中, 加入10 mL实验用水与四氟磁力搅拌子, 样品加热温度40 ℃, 经PT-GC/MS进行分析。结果 从34批次样品中, 共鉴定出260种风味物质, 涵盖含硫化合物、醇类、醛类、酮类、酯类等多种类型。生、熟豆汁中含硫化合物相对含量较高, 而麻豆腐的风味物质种类多样、相似性较低。这些鉴定数据在一定程度上能够反映感官评价结果, 但存在部分风味物质较为突出或被其他气味干扰的可能性。此外, 本研究利用主成分分析(principal component analysis, PCA)法对样品整体分布及偏离样本进行鉴别并尝试分析偏离原因; 进一步利用正交偏最小二乘判别分析(orthogonal partial least squares discriminant analysis, OPLS-DA), 基于[P<0.05, 变量投影重要性(variable importance in the projection, VIP)>1]的筛选条件, 选出31种生、熟豆汁特征风味物质, 可用于生、熟豆汁的区分与鉴定。结论 研究证实PT-GC/MS结合多元统计方法可有效解析豆汁、麻豆腐风味物质, 筛选特征物质, 为后续优化改善产品风味提供依据。

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杨志超(1984—), 男, 硕士, 工程师, 主要研究方向为食品质量与安全分析技术。E-mail:

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* 马立利(1981—), 女, 硕士, 副研究员, 主要研究方向为食品质量与安全分析技术。E-mail:
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杨志超(1984—), 男, 硕士, 工程师, 主要研究方向为食品质量与安全分析技术。E-mail:

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Journal of Chinese Institute of Food Science and Technology, 2013, 13(2): 199-204., articleTitle=The change of volatile aroma components of Douzhi in the heating process, refAbstract=null), Reference(id=1164258694712738449, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, doi=null, pmid=null, pmcid=null, year=2015, volume=36, issue=6, pageStart=103, pageEnd=108, url=null, language=null, rfNumber=[27], rfOrder=43, authorNames=卢晓丹, 张敏, 苗菁, journalName=食品科学, refType=null, unstructuredReference=卢晓丹, 张敏, 苗菁. 不同来源生熟北京豆汁的风味物质和感官评价比较[J]. 食品科学, 2015, 36(6): 103-108., articleTitle=不同来源生熟北京豆汁的风味物质和感官评价比较, refAbstract=null), Reference(id=1164258694775653011, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, doi=null, pmid=null, pmcid=null, year=2015, volume=36, issue=6, pageStart=103, pageEnd=108, url=null, language=null, rfNumber=[27], rfOrder=44, authorNames=LU XD, ZHANG M, MIAO J, journalName=Food Science, refType=null, unstructuredReference=LU XD, ZHANG M, MIAO J. Analysis of volatile compounds and sensory evaluation of different Douzhir (fermented mung bean juice) products[J]. Food Science, 2015, 36(6): 103-108., articleTitle=Analysis of volatile compounds and sensory evaluation of different Douzhir (fermented mung bean juice) products, refAbstract=null), Reference(id=1164258694838567572, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, doi=null, pmid=null, pmcid=null, year=2024, volume=40, issue=4, pageStart=34, pageEnd=39, url=null, language=null, rfNumber=[28], rfOrder=45, authorNames=陈璟, 任田, 赵子龙, journalName=食品与机械, refType=null, unstructuredReference=陈璟, 任田, 赵子龙, 等. 郫县豆瓣酱香气成分与感官评价[J]. 食品与机械, 2024, 40(4): 34-39., articleTitle=郫县豆瓣酱香气成分与感官评价, refAbstract=null), Reference(id=1164258694905676437, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, doi=null, pmid=null, pmcid=null, year=2024, volume=40, issue=4, pageStart=34, pageEnd=39, url=null, language=null, rfNumber=[28], rfOrder=46, authorNames=CHEN J, REN T, ZHAO ZL, journalName=Food & Machinery, refType=null, unstructuredReference=CHEN J, REN T, ZHAO ZL, et al. Aroma components and sensory evaluation of Pixian Douban sauce[J]. Food & Machinery, 2024, 40(4): 34-39., articleTitle=Aroma components and sensory evaluation of Pixian Douban sauce, refAbstract=null), Reference(id=1164258694976979605, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, doi=null, pmid=null, pmcid=null, year=2024, volume=null, issue=12, pageStart=180, pageEnd=187, url=null, language=null, rfNumber=[29], rfOrder=47, authorNames=陈召桂, 陈春梅, 姚远, journalName=中国粮油学报, refType=null, unstructuredReference=陈召桂, 陈春梅, 姚远, 等. 发酵米糕感官评价标准体系的建立[J]. 中国粮油学报, 2024(12): 180-187., articleTitle=发酵米糕感官评价标准体系的建立, refAbstract=null), Reference(id=1164258695044088470, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, doi=null, pmid=null, pmcid=null, year=2024, volume=null, issue=12, pageStart=180, pageEnd=187, url=null, language=null, rfNumber=[29], rfOrder=48, authorNames=CHEN ZG, CHEN CM, YAO Y, journalName=Journal of the Chinese Cereals and Oils Association, refType=null, unstructuredReference=CHEN ZG, CHEN CM, YAO Y, et al. Establishment of sensory evaluation standard system for fermented rice cake[J]. Journal of the Chinese Cereals and Oils Association, 2024(12): 180-187., articleTitle=Establishment of sensory evaluation standard system for fermented rice cake, refAbstract=null), Reference(id=1164258695098614424, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=https://pubchem.ncbi.nlm.nih.gov/, language=null, rfNumber=[30], rfOrder=49, authorNames=National center for biotechnology information, journalName=null, refType=null, unstructuredReference=National center for biotechnology information. PubChem[EB/OL].(2025-04-06)[2025-02-01]. https://pubchem.ncbi.nlm.nih.gov/, articleTitle=PubChem, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1167040876648870261, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, xref=1., ext=[AuthorCompanyExt(id=1167040876657258870, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, companyId=1167040876648870261, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. Institute of Analysis and Testing, Beijing Academy of Science and Technology (Beijing Center for Physical and Chemical Analysis), Beijing 100089, China), AuthorCompanyExt(id=1167040876665647479, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, companyId=1167040876648870261, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心), 北京 100089)]), AuthorCompany(id=1167040876715979128, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, xref=2., ext=[AuthorCompanyExt(id=1167040876728562041, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, companyId=1167040876715979128, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2. 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注: S为生豆汁, SH为熟豆汁, 图34同。

, figureFileSmall=MdYlIN6Cj4xApTlMdEYucw==, figureFileBig=BZ6RfyWZuQAbX4pnTw4XTw==, tableContent=null), ArticleFig(id=1167040879643603386, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, language=EN, label=Fig.3, caption=OPLS-DA and permutation retention of flavor compounds in raw and cooked Douzhir, figureFileSmall=MHQc5z7qKaH1s7S75BUPrg==, figureFileBig=2a3vD5fhB0iaH7adiuYesQ==, tableContent=null), ArticleFig(id=1167040879698129339, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, language=CN, label=图3, caption=生、熟豆汁风味物质的OPLS-DA和置换保留度

注: R2Q2用于评估模型可靠性和过拟合风险。

, figureFileSmall=MHQc5z7qKaH1s7S75BUPrg==, figureFileBig=2a3vD5fhB0iaH7adiuYesQ==, tableContent=null), ArticleFig(id=1167040879807181244, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, language=EN, label=Fig.4, caption=PCA of flavor compounds in raw and cooked Douzhir and Ma Tofu, figureFileSmall=pdQhOk+rZinTkNt8mB0SJQ==, figureFileBig=+MScEX5YJ2fDXexMksk8jg==, tableContent=null), ArticleFig(id=1167040879870095805, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, language=CN, label=图4, caption=生、熟豆汁和麻豆腐风味物质的PCA

注: M为麻豆腐。

, figureFileSmall=pdQhOk+rZinTkNt8mB0SJQ==, figureFileBig=+MScEX5YJ2fDXexMksk8jg==, tableContent=null), ArticleFig(id=1167040879949787582, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, language=EN, label=Table 1, caption=

Information of samples

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 生豆汁 熟豆汁 麻豆腐
样品编号 样品来源 样品编号 样品来源 样品编号 样品来源
1 1028016 GLSW 1028014 HSYSP 1028015 GLSW
2 1028017 HSYSP 1028019 LMHH 1028018 HSYSP
3 1028020 ZHSP 1028021 ZHSP 1028025 LMHH
4 1028022 HSYSP 1028024 LMHH 1028030 HSYSP
5 1028023 LMHH 1028027 HSYSP 1029003 HJLCQK
6 1028026 HSYSP 1028029 HSYSP 1029006 XDYY
7 1028028 HSYSP 1028031 XDYY 1029009 ZGHWJ
8 1029001 HJLCQK 1029002 HJLCQK 1030002 LHSP
9 1029005 ZHSP 1029004 ZHSP 1104003 XDYY
10 1029008 ZGHWJ 1029007 ZGHWJ - -
11 1030001 BYSM 1029010 YSDZ - -
12 1104001 XDYY 1029011 NJBJ - -
13 - - 1104002 XDYY - -
), ArticleFig(id=1167040880033673663, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1151437191097447023, language=CN, label=表1, caption=

样品信息

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 生豆汁 熟豆汁 麻豆腐
样品编号 样品来源 样品编号 样品来源 样品编号 样品来源
1 1028016 GLSW 1028014 HSYSP 1028015 GLSW
2 1028017 HSYSP 1028019 LMHH 1028018 HSYSP
3 1028020 ZHSP 1028021 ZHSP 1028025 LMHH
4 1028022 HSYSP 1028024 LMHH 1028030 HSYSP
5 1028023 LMHH 1028027 HSYSP 1029003 HJLCQK
6 1028026 HSYSP 1028029 HSYSP 1029006 XDYY
7 1028028 HSYSP 1028031 XDYY 1029009 ZGHWJ
8 1029001 HJLCQK 1029002 HJLCQK 1030002 LHSP
9 1029005 ZHSP 1029004 ZHSP 1104003 XDYY
10 1029008 ZGHWJ 1029007 ZGHWJ - -
11 1030001 BYSM 1029010 YSDZ - -
12 1104001 XDYY 1029011 NJBJ - -
13 - - 1104002 XDYY - -
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基于吹扫捕集-气相色谱/质谱法分析豆汁、麻豆腐中风味物质
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杨志超 1 , 梁颖 1 , 贾海先 2 , 李春雨 2 , 张春梅 1 , 马巧云 1 , 马晓晨 2 , 冯月超 1 , 邵鹏 1 , 马立利 1, *
食品安全质量检测学报 | 本期专题:食品风味研究 2025,16(11): 68-77
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食品安全质量检测学报 |本期专题:食品风味研究 2025 , 16 (11) : 68 -77
基于吹扫捕集-气相色谱/质谱法分析豆汁、麻豆腐中风味物质
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杨志超1 , 梁颖1, 贾海先2, 李春雨2, 张春梅1, 马巧云1, 马晓晨2, 冯月超1, 邵鹏1, 马立利1, *
作者信息
  • 1. 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心), 北京 100089
  • 2. 北京市疾病预防控制中心, 北京 100013
通讯作者:
* 马立利(1981—), 女, 硕士, 副研究员, 主要研究方向为食品质量与安全分析技术。E-mail:
Analysis of flavor compounds in Douzhir and Ma Tofu based on purge and trap-gas chromatography/mass spectrometry
Zhi-Chao YANG1 , Ying LIANG1, Hai-Xian JIA2, Chun-Yu LI2, Chun-Mei ZHANG1, Qiao-Yun MA1, Xiao-Chen MA2, Yue-Chao FENG1, Peng SHAO1, Li-Li MA1, *
Affiliations
  • 1. Institute of Analysis and Testing, Beijing Academy of Science and Technology (Beijing Center for Physical and Chemical Analysis), Beijing 100089, China
  • 2. Beijing Center for Disease Prevention and Control, Beijing 100013, China
出版时间: 2025-06-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250226004
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目的 基于吹扫捕集-气相色谱/质谱法(purge and trap-gas chromatography/mass spectrometry, PT-GC/MS)并结合美国国家标准与技术研究院(national institute of standards and technology, NIST)数据库, 鉴定豆汁、麻豆腐中的风味物质并分析其特征物质。方法 称取2.0 g样品, 于40 mL棕色螺旋样品瓶中, 加入10 mL实验用水与四氟磁力搅拌子, 样品加热温度40 ℃, 经PT-GC/MS进行分析。结果 从34批次样品中, 共鉴定出260种风味物质, 涵盖含硫化合物、醇类、醛类、酮类、酯类等多种类型。生、熟豆汁中含硫化合物相对含量较高, 而麻豆腐的风味物质种类多样、相似性较低。这些鉴定数据在一定程度上能够反映感官评价结果, 但存在部分风味物质较为突出或被其他气味干扰的可能性。此外, 本研究利用主成分分析(principal component analysis, PCA)法对样品整体分布及偏离样本进行鉴别并尝试分析偏离原因; 进一步利用正交偏最小二乘判别分析(orthogonal partial least squares discriminant analysis, OPLS-DA), 基于[P<0.05, 变量投影重要性(variable importance in the projection, VIP)>1]的筛选条件, 选出31种生、熟豆汁特征风味物质, 可用于生、熟豆汁的区分与鉴定。结论 研究证实PT-GC/MS结合多元统计方法可有效解析豆汁、麻豆腐风味物质, 筛选特征物质, 为后续优化改善产品风味提供依据。

豆汁  /  麻豆腐  /  吹扫捕集-气相色谱/质谱法  /  风味物质

Objective To identify flavor compounds in Douzhir and Ma Tofu and analyze their characteristic components based on purge and trap-gas chromatography/mass spectrometry (PT-GC/MS) combined with the national institute of standards and technology (NIST) database. Methods Weigh 2.0 g of sample into a 40 mL brown spiral sample bottle, add 10 mL of experimental water and a tetrafluoroethylene magnetic stirrer, heat the sample at 40 ℃, and analyze it by PT-GC/MS. Results A total of 260 kinds of flavor compounds were identified across 34 batches, including sulfur-containing compounds, alcohols, aldehydes, ketones, esters, etc. Raw and cooked Douzhir exhibited significantly higher relative abundances of sulfur-containing compounds compared to Ma Tofu, which showed greater diversity but lower similarity in flavor profiles. These identification data could to some extent reflect sensory evaluation results, but there was a possibility that some flavor compounds might be more prominent or interfered with by other odors. In addition, this study used principal component analysis (PCA) method to identify the overall distribution of samples and deviations from samples, and attempted to analyze the reasons for deviations. Further, using orthogonal partial least squares discriminant analysis (OPLS-DA), based on the screening conditions [P<0.05, variable importance in the projection (VIP)>1], 31 kinds of characteristic flavor compounds of raw and cooked Douzhir were selected, which could be used for the differentiation and identification of raw and cooked Douzhir. Conclusion The study confirms that PT-GC/MS combined with multivariate statistical method can effectively analyze the flavor compounds of Douzhir and Ma Tofu, screen the characteristic compounds, and provide a basis for the subsequent optimization and improvement of product flavor.

Douzhir  /  Ma Tofu  /  purge and trap-gas chromatography/mass spectrometry  /  flavor compounds
杨志超, 梁颖, 贾海先, 李春雨, 张春梅, 马巧云, 马晓晨, 冯月超, 邵鹏, 马立利. 基于吹扫捕集-气相色谱/质谱法分析豆汁、麻豆腐中风味物质. 食品安全质量检测学报, 2025 , 16 (11) : 68 -77 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250226004
Zhi-Chao YANG, Ying LIANG, Hai-Xian JIA, Chun-Yu LI, Chun-Mei ZHANG, Qiao-Yun MA, Xiao-Chen MA, Yue-Chao FENG, Peng SHAO, Li-Li MA. Analysis of flavor compounds in Douzhir and Ma Tofu based on purge and trap-gas chromatography/mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (11) : 68 -77 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250226004
豆汁是北京地区一种传统风味流食, 至今已有200多年历史。本为粉房做绿豆淀粉时生产的副产品, 用做淀粉的绿豆渣水发酵而成, 颜色灰绿, 汁味浓醇, 酸而微甜[1]。麻豆腐则为豆汁生产过程中的绿豆渣发酵而来, 具有独特的酸香味和豆香味[2]。随着互联网的发展, 不但吸引了大量外地游客来北京品尝[3], 还出现预包装产品上架线上平台和线下超市, 销量稳步提升。
经过文献调研[4-6]和对北京2家豆汁生产企业的调研发现, 各家企业的豆汁和麻豆腐制作工艺流程大致相同, 操作细节存在差异, 工艺流程如图1所示。
豆汁、麻豆腐的风味物质主要来自微生物的发酵[7-9], 但由于原材料的不同和自然发酵时优势菌的差别, 造成了各家豆汁、麻豆腐的风味差别。现阶段研究食品风味物质的方法主要有全二维气相色谱-飞行时间质谱技术[10-11]、固相微萃取/气相色谱-质谱技术[12-13]、吹扫捕集-气相色谱/质谱法(purge and trap-gas chromatography/mass spectrometry, PT-GC/MS)[14-17]、电子鼻+气相色谱-质谱法[18-19]的方式等。
PT技术是基于动态顶空原理, 通过惰性气体将痕量挥发性物质高效吹扫至捕集器, 其检出限相较于静态顶空显著提高。该技术前处理无需加入溶剂, 取样量较小。封闭式系统设计有效避免环境污染, 通过温度梯度控制可实现复杂基质中风味成分的无损提取[20]。近年研究显示, 该技术在食品风味指纹图谱构建、特征香气物质鉴定及加工过程风味演化研究方面展现出独特优势。如WU等[21]创新性地开发了一种微型化热辅助吹扫捕集装置(miniaturized thermal purge-and-trap, MTPT), 通过将葡萄酒中的二氧化硫(SO2)从液态基质中高效气化分离并富集, 显著提升了检测性能; 王璐等[16]采用PT-GC/MS快速测定生活饮用水中的82种挥发性有机物(volatile organic compounds, VOCs), 显著提高了痕量VOCs的富集效率; 李爱兰等[14]利用PT-GC/MS结合化学计量学, 鉴别不同产地和品牌的浓香型白酒。相较于静态顶空法, 该方法捕获的化合物种类更全面, 且无需复杂前处理。
本研究通过PT-GC/MS技术与多元统计方法[22-23], 构建豆汁、麻豆腐风味物质的分析框架, 建立正交偏最小二乘判别分析(orthogonal partial least squares discriminant analysis, OPLS-DA)[24]模型及特征物质数据库, 以期为实现生产过程精准监控与菌群定向调控提供依据。
前期调研发现, 北京市豆汁、麻豆腐的餐饮消费主要集中在东城、西城两个区, 其他城区消费量较小且分散。其中东城、西城以老字号为主, 而其他城区以连锁店为主。依据网络平台综合评分(≥4.0分)选取了5个城区20家消费者认可度较高、经营时间较长的餐饮机构进行采样, 分别为东城区7家、西城区6家、海淀区5家、朝阳区1家、丰台区1家。共购买34批次豆汁、麻豆腐样品, 包括12批次生豆汁、13批次熟豆汁和9批次麻豆腐。生豆汁样品来源除1029007样品为餐饮机构自制外, 其他均为生产企业生产; 熟豆汁样品来源除1029008样品为餐饮机构自制外, 其他样品均为生产企业生产、餐饮机构再加工; 麻豆腐样品来源均为生产企业生产。样品编号和样品来源(生产企业拼音缩写)如表1所示。
实验用水为屈臣氏蒸馏水(电阻率≥18.2MΩ·cm)、40 mL 棕色螺旋样品瓶(美国赛默飞公司); 内衬有聚四氟乙烯膜螺旋盖(美国CDS公司)。
BSA 224S天平(精度为0.1 mg, 德国赛多利斯公司); 7000E/7400吹扫捕集自动进样器(配5 mL砂芯式吹扫管, CDS7000E捕集阱, 美国CDS公司); GCMS-QP2010 Ultra气相色谱/质谱仪(日本岛津公司); DB-624毛细管色谱柱(60 m×0.25 mm, 1.40 μm)(美国安捷伦公司)。
称取2.0 g(精确至0.0001 g)豆汁、麻豆腐样品于40 mL 棕色螺旋样品瓶中, 加入10 mL蒸馏水, 加入四氟磁力搅拌子, 加盖拧紧, 运用仪器进行分析。
吹扫捕集条件: 吹脱气(高纯氮气), 流速40 mL/min, 吹扫时间11 min; 10#捕集阱, 解析预热温度245 ℃, 解析温度250 ℃, 烘焙温度265 ℃。解析时间3.0 min, 烘焙时间12 min, 样品加热温度40 ℃; 阀温180 ℃, 传输线温度180 ℃。
气相色谱条件: DB-624毛细管色谱柱(60 m×0.25 mm, 1.40 μm); 汽化室温度200 ℃, 分流进样, 分流比10:1 (V:V); 柱箱温度: 初温35 ℃, 保持5 min, 以10 ℃/min升至120 ℃, 不保持, 再以15 ℃/min升至240 ℃, 保持3.5 min。柱前压161.0 kPa。
质谱条件: 电子轰击(electron impact, EI)离子源温度230 ℃, 接口温度260 ℃; 电子倍增器电压1.2 kV, 扫描速度1111 amu/s, 扫描范围35~350 amu/s, 扫描时间3~25 min。
利用美国国家标准与技术研究院(national institute of standards and technology, NIST)数据库, 对样品的挥发性化合物进行质谱定性, 并利用总离子流图峰面积归一化法计算各化合物的相对含量。使用SIMCA 14.1软件进行主成分分析(principal component analysis, PCA)和OPLS-DA, 计算变量投影重要性(variable importance in the projection, VIP); 以P<0.05, VIP>1为条件筛选差异风味物质[25]
使用PT-GC/MS和NIST数据库, 鉴定出生、熟豆汁和麻豆腐中共有260种风味物质, 如表2所示。
12批次生豆汁共鉴定出134种风味物质, 含硫化合物共18种, 其中全部检出二甲基二硫醚、甲硫醇, 91.7%检出二甲基硫醚、环戊基甲基硫醚。甲基二硫醚和二甲基二硫醚的相对含量更高, 最大值分别可达到43.70%、41.88%。
生豆汁中醇类和酯类物质种类最丰富, 检出种类均为27种, 但每种物质的相对含量较低, 检出相对含量最大值较大的醇类物质如L-苏丁醇、正辛醇、3-甲基-1-戊醇也仅分别为18.81%、14.75%、10.19%, 酯类相对含量更是均小于10%。共有醇类和酯类物质为异丁醇、1-戊醇和乙酸丙酯3种。
酮类、醛类、烯烃、烷烃和其他类物质检出种类不多, 分别为11种、10种、8种、16种和15种, 全部样品均检出正己烷、正戊烷。1,2-二氟乙烷、甲基肼、(2R,3S)-2-甲基-3-戊基环氧乙烷、正辛醛、异丙基缩水甘油醚和丁醛的相对含量最大值较高, 分别为20.11%、19.92%、19.15%、16.99%、15.11%、13.00%, 其余相对含量均小于10%。
酸类物质检出较少, 仅有2种, β-甲基乙酰丙酸、甲酸检出率分别为25.0%、8.3%, 相对含量最大值分别为15.73%、19.87%。
生豆汁呈现出含硫化合物相对含量较高, 醇类和酯类物质种类最为丰富但单种含量普遍较低的特征。共有物质为甲硫醇、二甲基二硫醚、异丁醇、1-戊醇、乙酸丙酯、正戊烷、正己烷。
13批次熟豆汁共鉴定出121种风味物质, 其中含硫化合物共14种, 二甲基二硫醚和二甲基三硫醚为共有风味物质。与生豆汁类似, 甲基二硫醚、二甲基二硫醚的相对含量更高, 最大值可分别达到59.21%、41.23%。熟豆汁甲基二硫醚的检出率为23.1%, 低于生豆汁的41.7%。
熟豆汁中醇类物质种类最多, 共23种, 但每种物质的相对含量较低, 除正己醇的相对含量最大值为12.07%外, 其他均小于10%。共有物质有正己醇、叶醇和1-戊醇3种。
酮类、醛类、酯类、烯烃、烷烃和其他类物质检出种类分别为14种、14种、16种、4种、21种和15种, 其中全部检出2-丁酮、丙酮、正己醛、乙酸乙酯、正己烷。甲基肼、异丙基缩水甘油醚的相对含量最大值分别为41.04%、21.30%, 其余相对含量均小于10%。熟豆汁未检出酸类物质。
熟豆汁所含含硫化合物种类比生豆汁少, 可以说明通过熬煮的加工方式, 可以一定程度上减少含硫化合物, 起到除臭的作用。二甲基二硫醚、二甲基三硫醚、1-戊醇、正己醇、叶醇、丙酮、2-丁酮、乙酸乙酯、正己醛、正己烷为共有物质。
9批次麻豆腐共鉴定出185种风味物质, 其中含硫化合物共13种, 甲基二硫醚、二甲基二硫醚的相对含量较高, 最大值分别达到40.10%、22.47%。麻豆腐检出了34种酯类物质, 醇类和其他类物质也较多, 分别多达33种和31种。其中叶醇为共有物质。甲基肼的相对含量最大值较高, 为56.64%, 乙醇、仲丁醇、2-乙烯氧基乙醇、2-甲基-1,3-丙二醇、正己醇、3-甲基-1-戊醇、邻苯二甲酸单乙酯和邻苯二甲酸二乙酯的相对含量最大值分别为35.55%、17.60%、13.85%、16.49%、11.23%、22.87%、10.57%和12.62%, 其余相对含量均小于10%。
酮类、醛类、烯烃、烷烃检出种类分别为13种、17种、20种、23种, 异戊醛为共有物质。2-氯(正)己烷、正戊烷的相对含量最大值分别为20.90%、13.11%, 其余相对含量均小于10%。仅有一个样品鉴定出炔烃类物质, 3-壬炔的相对含量为0.18%。
麻豆腐的风味物质种类多于豆汁样品, 但含硫化合物相对含量最大值和检出率均较低。麻豆腐的共有化合物种类较少, 仅有叶醇、异戊醛两种。说明各家生产企业麻豆腐的生产工艺差别较大, 部分企业可能向产品中添加了其他辅料。
豆汁、麻豆腐的臭味主要来自二甲基二硫醚、二甲基三硫醚、甲硫醇等含硫化合物, 醇类、醛类、酮类、酯类等多种化合物可以提供青香、果香、甜香、醚香等丰富风味[26-27]。尝试将这些风味物质数据综合计算后, 与评价人员的主观感受对比[28-29]。如表3所示。
含硫化合物综合占比与感官评价的臭味强度评价成正相关, 检测结果能较好地反映感官评价结果。而豆香味组成复杂, 通过感官评价共筛选出17个豆香味呈适中或强的样本, 经过共性风味物质分析显示: 检出率≥70%的高频物质共16种, 如表4所示。推测这些化合物可能协同构成豆香味基底。进一步分析发现, 部分相对含量占比很大的物质对豆香特征可能存在掩蔽效应。例如, 样本1028030中乙醇含量高达35.54%, 其主导酒香风味可能干扰豆香味感知, 说明特征香气解析需综合考量化合物浓度、感官阈值及风味交互作用。
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通过SIMCA 14.1软件对生、熟豆汁中鉴定出的风味物质相对含量进行数据标准化处理后进行PCA, 分析结果显示, 生、熟豆汁间主成分基本能够区分, 可以有效反映样品间的差异特征。共有24批次样品数据处于置信区间内(95%以上), 置信区间外样品1028019共鉴定出68种风味物质, 显著高于另外12种熟豆汁鉴定出的39~57种。结果如图2所示。
从20家餐饮机构购买了12批次生豆汁、13批次熟豆汁, 且未从同一餐饮机构重复购买同类豆汁。12批次生豆汁中, 有2组同来源样品分别为: 1028017、1028022、1028026、1028028样品均来自HSYSP, 1028020、1029005样品均来自ZHSP。13批次熟豆汁中有12批次加工前为生产企业生产, 有4组同来源样品分别为: 1028014、1028027、1028029样品均来自HSYSP, 1028019、1028024样品均来自LMHH, 1028021、1029004样品均来自ZHSP, 1028031、1104002样品均来自XDYY, 如图2所示。
2组同来源生豆汁样品由于来自不同餐饮机构, 其存放条件与时间存在差异, 生豆汁样品后续发酵条件不同, 可能导致其风味物质有差异。4组同来源熟豆汁样品较生豆汁样品的差异更为显著。经调研了解到, 各餐饮机构对熟豆汁的加工工艺、熬煮时间和是否加入配料均有不同, 导致其风味差异更为显著。1029008生豆汁样品和1029007熟豆汁样品均来自同一家餐饮机构ZGHWJ, 1029008样品为该机构自制, 其风味物质与其他来自生产企业的生豆汁样品有较大差异。
1029008生豆汁样品中甲基二硫醚相对含量较高, 为43.70%。未鉴定出二甲基硫醚、环戊基甲基硫醚、3-戊醇等其他生豆汁均含有的风味物质, 其风味物质组成在生豆汁样品中具有显著的特殊性。基于此, 将该样品作为异常样品不参于整体分析, 有助于更清晰地体现生、熟豆汁间风味物质的差异特征。去除该数据后, 得到的OPLS-DA、置换保留度如图3所示。
OPLS-DA得分图中生豆汁分布在横轴的负半轴, 熟豆汁分布在横轴的正半轴呈现完全分离状态。为验证模型是否过拟合, 执行了200次置换检验(Y变量随机重排)。当Q2<0.05时证明模型拟合良好, 结果显示该模型的R2截距为0.734, Q2为-0.374均优于随机置换模型, 证明无过拟合风险。以P<0.05且VIP>1为标准, 筛选出24批次生、熟豆汁的差异风味物质有31种, 分别为: 戊醛、乙酸异戊酯、2-甲基丁醛、乙酸甲酯、壬醛、乙醛、庚醛、异戊醛、苯甲醛、甲基肼、异丁醛、2-已烯醛、1-戊烯、L-苏丁醇、甲硫醇、硫代乙酸甲酯、2-乙基己醇、反式-3-己烯-1-醇、1-戊醇、正己烷、2-己酮、苯、正戊烷、乙酸己酯、1-辛烯-3-醇、叶醇、丙酮、丙酸乙酯、2-乙基呋喃、2-丁酮、二甲基亚砜。
将麻豆腐的风味物质鉴定数据引入后, PCA结果显示, 麻豆腐样品在得分图中呈现显著分散分布(图4), 表明不同批次麻豆腐样品间风味物质组成存在较大异质性。9批次麻豆腐样品共鉴定出185种挥发性有机化合物, 其中仅叶醇、异戊醛为所有样品的共有成分。2批次麻豆腐样品未在置信区间内, 其中1029006样品检出86种风味物质,包含43种独有成分, 显著高于其他批次样品的44~62种检出量。1030002样品独有风味物质3-甲基-1-戊醇相对含量达到22.87%, 这一特征性成分可能是导致其风味独特的主要原因。上述结果表明, 尽管麻豆腐是豆汁生产过程中的副产物, 但由于其原料组成和发酵工艺的显著差异, 其风味物质成分更加复杂多样, 呈现出与豆汁截然不同的特征风味。
经鉴定, 二甲基二硫醚、甲硫醇、1-戊醇、异丁醇、乙酸丙酯、正己烷、正戊烷为生豆汁样品共有风味物质; 二甲基二硫醚、二甲基三硫醚、正己醇、叶醇、1-戊醇、2-丁酮、丙酮、正己醛、乙酸乙酯、正己烷为熟豆汁样品共有风味物质; 叶醇、异戊醛为麻豆腐样品共有风味物质。将鉴定结果进行PCA, 明显区分出生、熟豆汁的风味物质特征。基于P与VIP, 筛选出31种特征挥发性化合物, 可用于生、熟豆汁的区分与鉴定。麻豆腐样本的PCA揭示其风味呈现显著异质性, 主要源于加工工艺差异导致的风味物质构成差异。可利用销售数据构建消费偏好关联模型, 实现麻豆腐风味物质标准化, 破解“一店一味”“同名异味”的消费难题。
本研究采用PT-GC/MS在样品加热温度40 ℃下能够最大程度保留了样品特性, 有效捕集、鉴定豆汁、麻豆腐中的多种风味物质, 包括含硫化合物、醇类、醛类、酮类和酯类等。检测结果与感官评价对比分析, 可明确风味物质与感官体验的相关性, 在剔除潜在干扰物质后解析其呈味基底, 即可确定目标风味特征, 进而指导生产工艺与加工流程的优化升级。
豆汁、麻豆腐作为北京特色食品的典型代表, 受到人们越来越多的关注。如何能在继承和保留传统风味的基础上, 优化并开发出新口味的产品, 让更多消费者接受, 成为行业的重要发展方向。PT-GC/MS作为一种成本低廉、操作简便、可大批量检测的方法, 结合NIST数据库能够提供挥发性化合物CAS的特点, 建立数据库后, 可快速鉴定出目标化合物, 适用于需要大量、多波次、时效性强的检测需求, 对于豆汁类产品的风味改善研究具有现实意义。

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2025年第16卷第11期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250226004
  • 接收时间:2025-02-26
  • 首发时间:2025-07-14
  • 出版时间:2025-06-15
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  • 收稿日期:2025-02-26
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    1. 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心), 北京 100089
    2. 北京市疾病预防控制中心, 北京 100013

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* 马立利(1981—), 女, 硕士, 副研究员, 主要研究方向为食品质量与安全分析技术。E-mail:
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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

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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