Article(id=1261343849335668856, tenantId=1146029695717560320, journalId=1260987677001138203, issueId=1261336272929472630, articleNumber=null, orderNo=null, doi=10.13386/j.issn1002-0306.2025050181, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1747756800000, receivedDateStr=2025-05-21, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1778657408316, onlineDateStr=2026-05-13, pubDate=1777564800000, pubDateStr=2026-05-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1778657408316, onlineIssueDateStr=2026-05-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1778657408316, creator=13701087609, updateTime=1778657408316, updator=13701087609, issue=Issue{id=1261336272929472630, tenantId=1146029695717560320, journalId=1260987677001138203, year='2026', volume='47', issue='9', pageStart='1', pageEnd='504', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1778655601961, creator=13701087609, updateTime=1778657530282, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1261344361019728695, tenantId=1146029695717560320, journalId=1260987677001138203, issueId=1261336272929472630, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1261344361019728696, tenantId=1146029695717560320, journalId=1260987677001138203, issueId=1261336272929472630, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=363, endPage=369, ext={EN=ArticleExt(id=1261343857069965463, articleId=1261343849335668856, tenantId=1146029695717560320, journalId=1260987677001138203, language=EN, title=Preparation of High-stability Indicator Film Based on Oxalic Acid/Roselle Anthocyanin and Its Application in Monitoring the Freshness of Channel Catfish, columnId=1261343845820805453, journalTitle=Science and Technology of Food Industry, columnName=Storage and Preservation, runingTitle=null, highlight=null, articleAbstract=

This study developed a high-stability indicator film containing a roselle (Hibiscus sabdariffa) anthocyanin extract (RAE)-oxalic acid (OA) co-pigment indicator (RAO), investigated the stability of the RAO indicator and its effects on the structure and performance of the indicator film, and applied the film to monitor the freshness of channel catfish (Ictalurus punctatus). The results showed that the stability of the RAO indicator improved compared with single RAE indicator. Moreover, the film with the RAO indicator showed enhanced performance. The tensile strength and elongation at break of the indicator film increased from 16.10 MPa and 280.95% to 17.81 MPa and 349.45%, respectively. Its moisture content and water solubility decreased from 19.10% and 42.71% to 13.98% and 34.69%, respectively. Under conditions of 4 ℃, 45% humidity, and no light exposure, the RAO indicator film could be stored for up to 82 days (ΔE<5). When used for monitoring the freshness of channel catfish at 4 ℃, the indicator film changed from rose-red to yellow-gray as the fish spoiled, demonstrating its accuracy in monitoring the spoilage process and its great potential for freshness monitoring applications.

, correspAuthors=Saiyan CHEN, 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, authorCompany=null, fund=null, authors=null, authorsList=Hongdong DENG, Yang WANG, Chunyan JIANG, Zhengfeng FANG, Teng HUI, Saiyan CHEN), CN=ArticleExt(id=1261343877479448939, articleId=1261343849335668856, tenantId=1146029695717560320, journalId=1260987677001138203, language=CN, title=基于草酸/洛神花花青素的高稳定性指示膜制备及其在黔鱼新鲜度监测中的应用, columnId=1261343846517059923, journalTitle=食品工业科技, columnName=贮运保鲜, runingTitle=null, highlight=null, articleAbstract=

本研究开发了以草酸(Oxalic acid,OA)/洛神花花青素(Roselle anthocyanins extract,RAE)为共着色指示剂(RAO)的高稳定性指示膜,探究了RAO指示剂的稳定性及对指示膜结构和性能的影响,并应用于黔鱼新鲜度监测中。结果表明,相较于单一RAE指示剂,RAO指示剂的稳定性有所提高。同时,RAO指示膜的性能得到改善。拉伸强度和断裂伸长率分别从16.10 MPa、280.95%提高到17.81 MPa、349.45%;含水率和水溶失率均由19.10%和42.71%降低至13.98%和34.69%。在4 ℃温度、45%湿度且无光照条件下,RAO指示膜最长可贮藏82 d(ΔΕ<5)。将RAO指示膜应用于监测黔鱼新鲜度,发现在4 ℃时,随着黔鱼腐败变质,指示膜由玫红色变为黄灰色,表明该指示膜对新鲜黔鱼的变质腐败过程监测准确,在新鲜度监测方面的应用具有巨大潜力。

, correspAuthors=陈赛艳, authorNote=null, correspAuthorsNote=
陈赛艳(1983−),女,博士,讲师,研究方向:智能包装膜,E-mail:
, copyrightStatement=版权所有 © 2026《食品工业科技》编辑部, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=bm+/fr11SONO0XKtQUT+7w==, magXml=BU/wqop4U/yGOOrCGevttw==, pdfUrl=null, pdf=zn41xb8jv2k4YqS5jFClpA==, pdfFileSize=2160198, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=UXWEvQvUktXbVLDIJEDt7w==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=EX+insgKBvAZtm01xEu7eg==, mapNumber=null, authorCompany=null, fund=null, authors=

邓鸿东(2000−),男,硕士研究生,研究方向:智能包装膜,E-mail:

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邓鸿东(2000−),男,硕士研究生,研究方向:智能包装膜,E-mail:

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邓鸿东(2000−),男,硕士研究生,研究方向:智能包装膜,E-mail:

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refs=[Reference(id=1261343941824267188, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=null, journalName=null, refType=null, unstructuredReference=de OLIVEIRA F J G, BRAGA A R C, de OLIVEIRA B R, et al. 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Research progress of food freshness indicator packaging based on natural pigment[J]. Science and Technology of Food Industry, 2023, 44(3): 432−441., articleTitle=null, refAbstract=null), Reference(id=1261343961696878822, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[30], rfOrder=42, authorNames=null, journalName=null, refType=null, unstructuredReference=ENARU B, DREȚCANU G, POP T D, et al. Anthocyanins: Factors affecting their stability and degradation[J]. 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Research progress of environment-friendly packaging materials based on soy protein isolate[J]. Food and Fermentation Industries, 2019, 45(24): 269−277., articleTitle=null, refAbstract=null), Reference(id=1261343963265548547, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[32], rfOrder=45, authorNames=null, journalName=null, refType=null, unstructuredReference=BAO Yiwen, CUI Huijun, TIAN Jinlong, et al. Novel pH sensitivity and colorimetry-enhanced anthocyanin indicator films by chondroitin sulfate co-pigmentation for shrimp freshness monitoring[J]. Food Control, 2022, 131: 108441., articleTitle=null, refAbstract=null), Reference(id=1261343963668201736, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[33], rfOrder=46, authorNames=null, journalName=null, refType=null, unstructuredReference=EZATI P, PRIYADARSHI R, BANG Y J, et al. CMC and CNF-based intelligent pH-responsive color indicator films integrated with shikonin to monitor fish freshness[J]. Food Control, 2021, 126: 108046., articleTitle=null, refAbstract=null), Reference(id=1261343964217655569, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[34], rfOrder=47, authorNames=null, journalName=null, refType=null, unstructuredReference=ICMSF. Microorganisms in Foods 7: Microbiological Testing in Food Safety Management[M]. Berlin: Springer, 2011., articleTitle=null, refAbstract=null), Reference(id=1261343966142841120, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[35], rfOrder=48, authorNames=null, journalName=null, refType=null, unstructuredReference=韩林娜. 基于天然复合染料新鲜度指示膜的制备、性质及其在鳕鱼中的应用研究[D]. 沈阳: 沈阳师范大学, 2023., articleTitle=null, refAbstract=null), Reference(id=1261343966688100648, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[35], rfOrder=49, authorNames=null, journalName=null, refType=null, unstructuredReference=HAN Linna. Preparation, properties and indication of the membrane based on natural composite dye freshness its application research in cod[D]. Shenyang: Shenyang Normal University, 2023., articleTitle=null, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1261343880159609240, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, xref=null, ext=[AuthorCompanyExt(id=1261343880524513691, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, companyId=1261343880159609240, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=College of Food Science, Sichuan Agricultural University, Ya'an 625014, China), AuthorCompanyExt(id=1261343880994275741, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, companyId=1261343880159609240, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=四川农业大学食品学院,四川雅安 625014)])], figs=[ArticleFig(id=1261343929182634799, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, language=EN, label=Fig.1, caption=Absorbance of indicators under different storage conditions, figureFileSmall=zzeRWO67ZNGHb16eutB6Uw==, figureFileBig=UXWEvQvUktXbVLDIJEDt7w==, tableContent=null), ArticleFig(id=1261343930868745015, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, language=CN, label=图1, caption=不同贮藏条件下指示剂的吸光度

注:A图为RAO作指示剂,B图为RAE作指示剂。

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注:空白膜(a、d);RAE膜(b、e);RAO膜(c、f)。

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Chromaticity of indictors before and after being stored for 30 days under different conditions

, figureFileSmall=null, figureFileBig=null, tableContent=
样品贮藏条件L*a*b*ΔΕ
注:不同小写字母表示不同组别样品之间存在显著差异(P<0.05),表2同。
RAE贮藏前44.67±1.52d46.33±2.51ab17.00±2.00c
66.00±1.73a5.67±1.52c21.67±3.21b46.25±1.75a
56.00±2.00b43.30±0.57b18.33±1.52c11.88±1.95b
RAO贮藏前42.33±2.08d49.00±1.00a29.00±1.00a
48.67±1.52c47.00±3.46ab22.67±0.57b8.06±0.24c
43.00±2.00d48.00±2.64a22.00±1.00b5.04±0.13d
), ArticleFig(id=1261343940721165207, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, language=CN, label=表1, caption=

指示剂在不同条件下贮藏30 d前后的色度值

, figureFileSmall=null, figureFileBig=null, tableContent=
样品贮藏条件L*a*b*ΔΕ
注:不同小写字母表示不同组别样品之间存在显著差异(P<0.05),表2同。
RAE贮藏前44.67±1.52d46.33±2.51ab17.00±2.00c
66.00±1.73a5.67±1.52c21.67±3.21b46.25±1.75a
56.00±2.00b43.30±0.57b18.33±1.52c11.88±1.95b
RAO贮藏前42.33±2.08d49.00±1.00a29.00±1.00a
48.67±1.52c47.00±3.46ab22.67±0.57b8.06±0.24c
43.00±2.00d48.00±2.64a22.00±1.00b5.04±0.13d
), ArticleFig(id=1261343941090263967, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, language=EN, label=Table 2, caption=

Results of film thickness, mechanical properties, moisture content and water solubility loss rate

, figureFileSmall=null, figureFileBig=null, tableContent=
样品厚度(cm)拉伸强度(MPa)断裂伸长率(%)含水率(%)水溶失率(%)
空白膜0.047±0.034c14.30±0.438b231.13±8.86c11.67±0.42c38.88±0.17b
RAE指示膜0.061±0.025b16.10±0.72ab280.95±12.02b19.10±0.34a42.71±0.71a
RAO指示膜0.063±0.021a17.81±0.58a349.45±6.92a13.98±1.61b34.69±0.62c
), ArticleFig(id=1261343941434196903, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1261343849335668856, language=CN, label=表2, caption=

膜的厚度、力学性能、含水率和水溶失率结果

, figureFileSmall=null, figureFileBig=null, tableContent=
样品厚度(cm)拉伸强度(MPa)断裂伸长率(%)含水率(%)水溶失率(%)
空白膜0.047±0.034c14.30±0.438b231.13±8.86c11.67±0.42c38.88±0.17b
RAE指示膜0.061±0.025b16.10±0.72ab280.95±12.02b19.10±0.34a42.71±0.71a
RAO指示膜0.063±0.021a17.81±0.58a349.45±6.92a13.98±1.61b34.69±0.62c
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基于草酸/洛神花花青素的高稳定性指示膜制备及其在黔鱼新鲜度监测中的应用
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邓鸿东 , 王杨 , 江春燕 , 方正锋 , 惠腾 , 陈赛艳 *
食品工业科技 | 贮运保鲜 2026,47(9): 363-369
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食品工业科技 | 贮运保鲜 2026, 47(9): 363-369
基于草酸/洛神花花青素的高稳定性指示膜制备及其在黔鱼新鲜度监测中的应用
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邓鸿东 , 王杨, 江春燕, 方正锋, 惠腾, 陈赛艳*
作者信息
  • 四川农业大学食品学院,四川雅安 625014
  • 邓鸿东(2000−),男,硕士研究生,研究方向:智能包装膜,E-mail:

通讯作者:

陈赛艳(1983−),女,博士,讲师,研究方向:智能包装膜,E-mail:
Preparation of High-stability Indicator Film Based on Oxalic Acid/Roselle Anthocyanin and Its Application in Monitoring the Freshness of Channel Catfish
Hongdong DENG , Yang WANG, Chunyan JIANG, Zhengfeng FANG, Teng HUI, Saiyan CHEN*
Affiliations
  • College of Food Science, Sichuan Agricultural University, Ya'an 625014, China
出版时间: 2026-05-01 doi: 10.13386/j.issn1002-0306.2025050181
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本研究开发了以草酸(Oxalic acid,OA)/洛神花花青素(Roselle anthocyanins extract,RAE)为共着色指示剂(RAO)的高稳定性指示膜,探究了RAO指示剂的稳定性及对指示膜结构和性能的影响,并应用于黔鱼新鲜度监测中。结果表明,相较于单一RAE指示剂,RAO指示剂的稳定性有所提高。同时,RAO指示膜的性能得到改善。拉伸强度和断裂伸长率分别从16.10 MPa、280.95%提高到17.81 MPa、349.45%;含水率和水溶失率均由19.10%和42.71%降低至13.98%和34.69%。在4 ℃温度、45%湿度且无光照条件下,RAO指示膜最长可贮藏82 d(ΔΕ<5)。将RAO指示膜应用于监测黔鱼新鲜度,发现在4 ℃时,随着黔鱼腐败变质,指示膜由玫红色变为黄灰色,表明该指示膜对新鲜黔鱼的变质腐败过程监测准确,在新鲜度监测方面的应用具有巨大潜力。

洛神花花青素  /  草酸  /  共着色  /  高稳定性指示膜

This study developed a high-stability indicator film containing a roselle (Hibiscus sabdariffa) anthocyanin extract (RAE)-oxalic acid (OA) co-pigment indicator (RAO), investigated the stability of the RAO indicator and its effects on the structure and performance of the indicator film, and applied the film to monitor the freshness of channel catfish (Ictalurus punctatus). The results showed that the stability of the RAO indicator improved compared with single RAE indicator. Moreover, the film with the RAO indicator showed enhanced performance. The tensile strength and elongation at break of the indicator film increased from 16.10 MPa and 280.95% to 17.81 MPa and 349.45%, respectively. Its moisture content and water solubility decreased from 19.10% and 42.71% to 13.98% and 34.69%, respectively. Under conditions of 4 ℃, 45% humidity, and no light exposure, the RAO indicator film could be stored for up to 82 days (ΔE<5). When used for monitoring the freshness of channel catfish at 4 ℃, the indicator film changed from rose-red to yellow-gray as the fish spoiled, demonstrating its accuracy in monitoring the spoilage process and its great potential for freshness monitoring applications.

roselle anthocyanin  /  oxalic acid  /  co-pigmentation  /  high-stability indicator film
邓鸿东, 王杨, 江春燕, 方正锋, 惠腾, 陈赛艳. 基于草酸/洛神花花青素的高稳定性指示膜制备及其在黔鱼新鲜度监测中的应用. 食品工业科技, 2026 , 47 (9) : 363 -369 . DOI: 10.13386/j.issn1002-0306.2025050181
Hongdong DENG, Yang WANG, Chunyan JIANG, Zhengfeng FANG, Teng HUI, Saiyan CHEN. Preparation of High-stability Indicator Film Based on Oxalic Acid/Roselle Anthocyanin and Its Application in Monitoring the Freshness of Channel Catfish[J]. Science and Technology of Food Industry, 2026 , 47 (9) : 363 -369 . DOI: 10.13386/j.issn1002-0306.2025050181
花青素因其来源广泛、生物相容性高且对pH变化敏感(在酸性条件下呈红色,中性至碱性条件下逐渐变为蓝色或绿色)而被广泛应用于指示膜的研究开发中[1]。洛神花花青素(Roselle anthocyanins extract,RAE)在花萼中含量丰富,常作为天然色素应用于食品新鲜度指示中。本课题组前期曾采用洛神花花青素制备指示膜,在巴沙鱼肉的新鲜度监测中应用效果良好[2]。也有研究者将洛神花花青素制备成指示膜用于鸡里脊肉新鲜度监测,发现指示膜表现出可视化的色差[3]。还有学者将酰基化的花青素制备指示膜并用于牛肉新鲜度监测,取得良好效果[4]。这些研究现状表明,洛神花花青素在食品新鲜度监测中应用潜力较大。洛神花花青素的主要成分为飞燕草素-3-O-半乳糖苷、矢车菊素-3-O-半乳糖苷、飞燕草素-3-O-葡萄糖苷、矢车菊素-3-桑布双糖苷与飞燕草素-3-桑布双糖苷,各成分中均含有大量羟基,导致其稳定性较差,易受环境因素影响而应用受限,故提高花青素的稳定性,扩大其在指示膜及食品新鲜度监测中的应用势在必行。
目前有研究者通过包埋花青素制备皮克林乳液[56]等方式提高花青素的稳定性,但包埋易降低花青素的pH敏感性,导致花青素对食品新鲜度监测响应迟钝。乳液法则对固体颗粒(如二氧化硅、纤维素纳米晶体等)的润湿性能依赖较强,且由于花青素的易溶于水的特性而难于控制水乳平衡。共着色是通过花青素分子与共着色剂通过分子间、分子内、自聚合以及金属络合[7]方式结合而增强和保护黄酮阳离子,提高花青素的颜色稳定性。常用的共着色剂主要包括酚类化合物、生物聚合物和金属离子等。其中,安全无毒、易于获得且价格便宜的有机酸(如单宁酸、柠檬酸、乙酸等)最受研究者青睐,而草酸(Oxalic acid,OA)因其辅色效果和适用性俱佳更备受重视。蒋新龙等[8]研究发现,草酸作为共着色剂有利于提高黑豆种皮花色苷在光热处理条件下的稳定性,扩大其应用及保存价值。Huang等[9]将草酸与洛神花花青素共着色,发现草酸有效提高了花青素的稳定性。故本研究选择草酸作为共着色剂提高花青素的稳定性,具有一定的理论基础。
聚乙烯醇(Polyvinyl alcohol,PVA)具有优异的成膜性和生物降解性,成膜后具有良好透明度、无毒性和阻隔性,但PVA的亲水性可能使膜材料在高湿度环境中过度溶胀,且成膜后脆性较大[10]。羟丙基纤维素(Hydroxypropyl cellulose,HPC)的引入可改善膜的柔韧性,降低聚乙烯醇的过度溶胀,且HPC与PVA通过分子链间的氢键网络增强膜的机械性能和耐水性能[1112]。本课题组前期将HPC与PVA结合制备成复合膜,并添加共着色指示剂制备成指示膜,发现HPC、PVA与花青素共着色指示剂的结合良好[13],故本研究的理论基础较强。但目前的研究缺乏对共着色剂用量对指示膜性能尤其是稳定性的影响。
本研究以OA为共着色剂,通过共着色方式制备RAO共着色指示剂,以PVA和HPC为复合基材,采用流延法制备高稳定性指示膜。研究分析了RAO指示剂的稳定性,探讨了指示剂用量对指示膜的机械性能、耐水性能、pH敏感性和颜色稳定性的影响。并将指示膜应用于黔鱼新鲜度监测中,分析了黔鱼腐败过程中指示膜的颜色变化过程,为开发高稳定性的共着色指示剂和指示膜提供了理论依据与技术参考。
洛神花 广东肇庆提供;黔鱼 四川雅安;无水乙醇、草酸 分析纯,四川成都金山化学试剂有限公司;聚乙烯醇1799 分析纯,成都市科隆化学品有限公司;羟丙基纤维素 纯度97%,上海皓鸿生物医药科技有限公司;超纯水 实验室自制。
CR400色差仪 柯尼卡美能达;KDN-520自动凯氏定氮仪 杭州旌斐仪器科技有限公司;Nicolet-6700傅里叶变换红外光谱仪 美国ThermoFisher;UV-756CRT型紫外可见分光光度计 聚仪惠供应链青岛有限公司;RE-201D型旋转蒸发仪 郑州特尔仪器设备有限公司。
将洛神花干燥至恒定重量,研磨成粉末,最终通过60目筛。每10 g洛神花粉末溶解于100 mL 50%乙醇中,在30 ℃加热4 h后过滤,在40 ℃的黑暗中使用真空旋转蒸发器浓缩至20±2 mL。样品最终在−18 ℃下冷冻,随后真空冷冻干燥2 d,得到花青素提取物。这些提取物随后储存在黑暗−20 ℃中,备用。
参考Jiang等[13]的方法并做调整,将0.08 g OA和0.16 g RAE(mOA:mRAE=1:2)混合溶于100 mL超纯水中,超声5 min,超声功率360 W,获得RAO指示剂。将指示剂均分成2份。一份在4 ℃下保存,一份真空冷冻干燥48 h,于4 ℃下保存,备用。
指示剂的稳定性采用吸光度值变化(降解率)和表观色度变化共同表示。降解率越高,表示指示剂的稳定性越低。分别将0.24 g RAO和RAE溶于100 mL超纯水中,并均匀分成两份,贮藏于不同条件下:a.室温25 ℃、室湿45%、见光;b.室温25 ℃、室湿45%、避光。在0 d和30 d通过iPhone13手机对贮藏前后的溶液进行拍照,利用Adobe Photoshop 2023获得贮藏前后的L*a*b*,通过公式(1)计算总色差(ΔE)。其中,L*a*b*为贮藏后溶液的色度值,L0*a0*b0*为贮藏前溶液的色度值。
$ {\Delta }E=\sqrt{{({L}^{\text{*}}-L_{0}^{\text{*}})}^{2}+{({a}^{\text{*}}-a_{0}^{\text{*}})}^{2}+{({b}^{\text{*}}-b_{0}^{\text{*}})}^{2}} $
利用紫外-可见分光光度计在400~700 nm范围内测试溶液的紫外-可见光光谱[1314]并计算降解率。其中A0为初始溶液的吸光度值,A1为放置后溶液的吸光度值。
$\rm \text{降解率}(\text{%})=\frac{{A}_{0}-{A}_{1}}{{A}_{0}}\times 100 $
参考Jiang等[13]的研究,将2.4 g PVA溶于100 mL超纯水中,95 ℃下搅拌30 min,得到PVA溶液。加入0.6 g HPC,30 ℃下搅拌2 h。加入RAO指示剂(0.24%,w/v,mOA:mRAE=1:2),搅拌2 h。对所得溶液进行超声脱气处理直至无气泡,得到成膜液。RAO指示膜(9 cm×9 cm)通过溶剂浇铸法显影,并在烘箱中干燥24 h (40 ℃)。以加入未添加OA稳定剂的洛神花花青素作为指示剂的指示膜为对照膜,记为RAE膜;以不添加指示剂的膜为空白膜。
膜样品在液氮中淬断,固定在样品台上喷金,观察样品表面形貌,放大3000倍和5000倍,加速电压为5 kV。
将薄膜烘至绝干,研磨,与绝干状态的溴化钾以质量比m:m溴化钾=7:3混合研磨,压片,检测,分析。扫描范围4000~500 cm−1,扫描次数32次,分辨率为2 cm−1[15]
用数显千分尺,在每张膜上随机选取6个点以测定膜的厚度。指示膜被切割成条状(10 cm×1 cm),并固定在拉伸分析仪上,初始距离为40 mm,拉伸速度为25 mm/min,直至拉断。重复3次。
将0.5 g膜在高温下(105 ℃)干燥至恒重。其中,M1为初始膜质量(g),M2为膜最终质量(g)。
$\rm \text{含水率}(\text{%})=\frac{{M}_{1}-{M}_{2}}{{M}_{1}}\times 100 $
在室温下,将0.5 g膜浸泡于50 mL蒸馏水中持续振荡24 h。之后,在105 ℃下干燥至恒重。其中,W0为指示膜初始质量(g),W1为指示膜最终质量(g)。
$\rm \text{水溶失率}(\text{%})=\frac{{W}_{0}-{W}_{1}}{{W}_{0}}\times 100 $
将指示膜(2 cm×2 cm)贮藏在不同条件下,使用色差仪测试指示膜的色度值,并计算色差,以色差变化表示颜色稳定性。从15 d开始每隔15 d测试一次色度值,测至90 d,每个样品需重复测定 3 次。贮藏条件:a.室温25 ℃,室湿45%和75%;b.室温25 ℃、室湿45%,光照和避光;c.室湿45%无光,温度4 ℃和25 ℃。色度与色差的计算见公式(1)。
将1.5±0.2 kg黔鱼剖开,处理内脏,洗净,切片,每块鱼片重量30±1 g,厚度5±0.1 mm。紫外灯杀菌后立刻放入无菌培养皿中,将指示膜置于顶部,在4 ℃培养箱中保存6 d。
通过iPhone13手机拍照,利用 Photoshop 2023获取指示膜的色度值。
向5 g黔鱼肉糜中加入45 mL蒸馏水,以10000 r/min匀浆2 min, 4 ℃,8000 r/min离心10 min,获得上清液,测定pH。
参照GB 5009.228-2016[16]和GB 4789.2-2022[17]进行测定。
所有实验均重复3次,结果用平均值±标准差表示。采用SPSS 23.0软件进行单因素方差分析(ANOVA)和Duncan多重检验,P<0.05表示差异具有显著性。采用Origin 2021进行绘图分析。
花青素随着时间的推移发生降解,主要的降解机制是氧化和水解[18]。将OA加入到RAE溶液中产生共着色效应以提高稳定性。在520 nm处的吸光度能够反映花青素含量,因此RAE与OA共着色后,对花青素稳定性的影响以吸光度值指标评价。如图1所示,在不同条件下贮藏15 d,RAE的吸光度值下降了18.90%(暗)和50.71%(光),而RAO的吸光度值下降了4.5%(暗)和7.74%(光)。在可见光条件下贮藏30 d后,RAE指示剂的花青素降解率高达72.63%,而RAO降解率仅为9.50%。这是因为RAO通过共着色作用形成致密的三明治结构可以抵抗花青素的降解[7],因此RAO指示剂表现出更高的稳定性。
色度是评价花青素稳定性最直观的指标。将RAE指示剂和RAO指示剂分别置于不同条件下贮藏30 d,色度如表1所示。加入OA后RAE溶液的初始红色度无显著差异,但贮藏30 d后的红色度显著增强,表明OA有助于RAE的显色。RAE指示剂溶液在见光和避光条件下的ΔΕ均大于5,其中在见光条件下RAE指示剂溶液的ΔΕ为46.25,而RAO在避光条件下保存30 d的ΔΕ为5.04,因此RAO指示剂表现出更高的稳定性。Fan等[19]在研究阿魏酸和黑莓花青素共着色增稳效果时发现阿魏酸能够更好地保持黑莓花青素的颜色参数,与本研究结果类似。
空白膜、RAE膜和RAO膜的表面和横截面如图2所示。由图2可知,空白膜表面平整,未出现孔洞和片状结构,横截面致密,说明PVA和HPC之间相容性良好。加入RAE及RAO之后,薄膜的横截面仍然致密,表明成膜基材和RAE及RAO的相容性均良好。但加入RAO指示剂之后的薄膜表面呈现粗糙、不平整,可能是过量指示剂在膜表面停留。除此之外,横截面中可以看出有非常微小的裂纹和空洞,这些空腔可能是干燥过程中水分迁移至表面而形成的[20]
为研究指示膜的官能团及分子相互作用,采用红外光谱进行分析,结果如图3所示。其中3500~3000 cm−1附近的宽峰为O-H伸缩振动,可能来自羟丙基纤维素和聚乙烯醇,而2930 cm−1附近的特征峰对应于C-H伸缩振动[21]。同时,RAE的吡喃环、芳香环、芳香烃骨架的C=C和C-O-C伸缩振动分别位于 1637、1425和1068 cm−1附近[22]。1327 cm−1的C-O伸缩振动峰增强,可能是羟基的引入使得分子间相互作用增加。整个红外图未发现在指示膜中生成新的吸收峰,表明在RAE膜和RAO膜中未生成新的官能团,各成分为物理混合,这与SEM结果一致。与RAE指示膜相比,引入OA后,RAO指示膜中3500~3000 cm−1的O-H伸缩振动明显向低波数偏移,表明共着色指示剂中形成了氢键。1068 cm−1附近的峰的减弱和移动,可能是由于分子相互作用或重组[5]
指示膜的拉伸强度、断裂伸长率和厚度如表2所示。其中,空白膜的厚度最小(0.047 cm),加入RAE后指示膜厚度有所增加(0.061 cm), RAO指示膜的厚度最大(0.063 cm),可能是溶质增加所致。
在引入RAE后,膜的拉伸强度值增加,可能是因为膜组分之间相互作用产生了氢键,增加了抗断裂能力[23]。RAO指示膜的拉伸强度值最高(17.81±0.58 MPa),可能是产生了更多的氢键和非共价键,使膜的抗断裂能力略强于RAE指示膜。在含有蓝莓花青素的指示膜中也得到了类似的结果[23]
加入OA共着色后,指示膜的断裂伸长率值从280.95%±12.02%(RAE指示膜)增加到349.45%±6.92%(RAO指示膜),表明柔韧性增加,这可能归因于加入OA后增强了膜组分间的相容性和分子间的有序排列。通常拉伸强度越高,拉伸断裂率越低,但在三组膜中拉伸强度增加的同时,拉伸断裂率也有所增加,可能是因为羟丙基纤维素具有增加强度、稠度以及提高膜内的分子排列有序性的作用[24]
含水率与水溶失率是基于生物聚合物制备而成的指示膜的重要功能特性[25]。在指示膜的应用过程中,水溶失率影响指示膜的完整性。如表2所示,空白膜的含水率为11.67%,水溶失率为38.88%。加入RAE后含水率增加(19.10%),这是由于RAE分子链中含有丰富的亲水性羟基。同时RAE指示膜表现出相对较高的水溶失率(42.71%),这是因为花青素是一种极强的水溶性物质,在Alizadeh-sani等[26]的研究中也观察到类似的现象。而在 RAO膜中,RAE与OA的共着色作用使RAO指示膜的含水率、水溶失率显著降低(P<0.05),分别为13.98%、34.69%,这是因为OA的引入产生了较强的分子间相互作用(氢键、静电作用),提高了花青素的稳定性,导致指示膜的水溶失率降低,在图3发生的波峰红移和相关研究中都印证了这一点[25,27]
花色苷的稳定性易受多种因素(如温度、光照和湿度)的影响而发生颜色变化[18,2830]。指示膜中的花色苷自身颜色变化影响食品新鲜度监测的准确性,因此指示膜的颜色稳定性对监测性能至关重要。本研究评估了RAE膜和RAO膜在不同条件下贮存90 d后色度值的变化,如图4所示,其中室温和室湿的条件分别是室温22±2℃,室湿75%RH。
当薄膜的色差(ΔE)大于5时,薄膜显示出肉眼可见的颜色变化[31]。RAO膜出现色差值ΔΕ大于5的时间节点分别为82 d(图4C)和75 d(图4B),RAE膜在45 d和35 d时ΔΕ大于5。在见光时,RAE膜在15 d时ΔE为8.15,而RAO膜在75 d后ΔE>5。90 d后RAO膜和RAE膜的ΔE值分别为12.16和21.73。在室湿45%和75%的处理条件下,RAO膜在75 d后和30 d后ΔE>5, 90 d后RAO膜的ΔE值远小于RAE膜的ΔE值。
由此可见,与RAE膜相比,RAO膜在上述储存条件下均表现出优异的颜色稳定性,OA与RAE之间的共着色效应有效提高了花色苷的颜色稳定性。Bao等[32]也发现了类似结果。因此,RAO膜在食品包装应用中具有巨大潜力。从图中色差数据来看,温度对指示膜的颜色稳定性影响较小,而湿度的影响最大,在后续贮藏中更应注意湿度和光照条件的严格控制。
鱼肉初始pH在6.45左右,随着贮藏时间延长,第2 d时鱼肉的pH下降至6.22,是因为ATP 酶、糖类酵解及乳酸菌等作用产生乳酸[33]。后续贮藏时间中pH均上升,是由于蛋白质分解产生碱性胺类物质。鱼肉的TVC值变化如图5A所示。第0~3 d,鱼肉的TVC值保持在3.64~5.17 lg(CFU/g),表明鲜切黔鱼此时还是新鲜可食的。根据国际食品微生物标准委员会(ICMSF,2011年)发布的《Microorganisms in Foods 7: Microbiological Testing in Food Safety Management》规范[34],新鲜鱼的初始TVC、合格临界值和可容受上限分别为2~5、 5.7 和7 lg(CFU/g),将实验TVC值限量设为 6 lg(CFU/g)。鱼肉在第4 d的TVC值超过标准(达到7.10 lg (CFU/g)),表明鱼肉此时不宜食用。GB 2733-2015《食品安全国家标准 鲜、冻动物性水产品》规定,淡水鱼的TVB-N含量≤20 mg/100 g时被认为是可接受的。将鱼肉储存在4 ℃下,初始TVB-N值为8.15 mg/100 g。第3 d时,鱼肉的TVB-N值(18.49 mg/100 g)接近于可接受值,说明此时的鱼肉即将腐败变质。4 d后鱼肉TVB-N值(24.19 mg/100 g)超过标准所规定的可接受值,说明鱼肉完全腐败,不宜食用。
贮藏6 d的监测照片如图5所示。根据上述TVC、pH 和TVB-N的研究结果可知,鲜切黔鱼在0~2 d是新鲜的,第3 d接近腐败,4~5 d腐败变质,在第6 d已完全腐败变质。RAO膜的颜色也由最开始的玫红色变为浅玫红色(0~2 d),红色变淡(3 d),发灰(4 d),偏黄(5 d),黄灰色(6 d)。同时,第4 d样品鱼肉中的蛋白质分解、细菌污染等导致碱性气体增加[35];第5 d时,鱼肉开始变黄;第6 d时,鱼肉变黄,表面出现黏液,完全腐败。由此可见,在鲜切黔鱼的应用中指示膜具有肉眼可见的颜色响应,能够很好地分辨、监测鱼肉的腐败程度,该指示膜在水产品新鲜度监测中具有应用潜力。
OA对RAE的共着色作用是一种很有前景的提高天然花青素稳定性的策略,本研究发现OA的加入能有效稳定RAE指示剂,其指示膜在贮藏80 d后仍表现出较高的稳定性。RAO指示剂与成膜基材(聚乙烯醇、羟丙基纤维素)相容性良好,指示膜有高于RAE膜的机械性能和疏水性能。将RAO指示膜应用于鲜切黔鱼新鲜度监测中时,发现4 ℃、冷藏条件下,鲜切黔鱼在第4 d已完全不可食用时,指示膜的颜色由玫红色变为渐渐发灰,过程中指示膜的颜色与TVC、TVB-N等增长趋势相关,能较为准确地监测并指示黔鱼的新鲜度。综上所述,RAO指示膜在监测黔鱼新鲜度方面具有巨大潜力。
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2026年第47卷第9期
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doi: 10.13386/j.issn1002-0306.2025050181
  • 接收时间:2025-05-21
  • 首发时间:2026-05-13
  • 出版时间:2026-05-01
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  • 收稿日期:2025-05-21
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    四川农业大学食品学院,四川雅安 625014

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陈赛艳(1983−),女,博士,讲师,研究方向:智能包装膜,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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