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Article(id=1217845646913094647, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20250319001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1742313600000, receivedDateStr=2025-03-19, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768286628702, onlineDateStr=2026-01-13, pubDate=1756051200000, pubDateStr=2025-08-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768286628702, onlineIssueDateStr=2026-01-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768286628702, creator=13701087609, updateTime=1768286628702, updator=13701087609, issue=Issue{id=1217845635080962613, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='16', pageStart='1', pageEnd='324', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=null, createTime=1768286625881, creator=13701087609, updateTime=1768287480278, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1217849218753024879, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1217849218753024880, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1217845635080962613, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=297, endPage=303, ext={EN=ArticleExt(id=1217845647861006425, articleId=1217845646913094647, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Optimization of caffeine removal process in green tea by supercritical carbon dioxide extraction, columnId=1151895321719223288, journalTitle=Journal of Food Safety & Quality, columnName=Food Processing and Technology, runingTitle=null, highlight=null, articleAbstract=

Objective To explore the process of caffeine removal from green tea by supercritical carbon dioxide extraction. Methods Using Wuyuan green tea as raw material, supercritical carbon dioxide extraction was used to remove caffeine from green tea. Taking the caffeine removal rate as the investigation index, the effects of tea moisture content, extraction temperature, pressure, time, concentration and dosage of entrained agent on caffeine removal rate were studied by single factor experiment, and the caffeine removal process was optimized by orthogonal experiment. Results The optimal extraction process of caffeine removal in green tea was tea moisture content 40%, extraction pressure 30 MPa, extraction temperature 55 ℃, extraction time 240 min, concentration of entrainment agent (ethanol) 60%, and dosage of entrainment agent 1.2:1 (m:m). Under these conditions, the caffeine removal rate was 91.2%. Extraction pressure was the most important factor affecting caffeine removal rate, followed by extraction temperature, and extraction time had relatively little effect. Conclusion This study determines the best technology of caffeine removal in green tea by supercritical carbon dioxide extraction, which provides a certain reference for caffeine removal in green tea.

, correspAuthors=Xiao-Hua LIU, 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, authorCompany=null, fund=null, authors=null, authorsList=Wen-Wen XU, Lin-Yue QI, Hui-Liang XU, Xiao-Hua LIU), CN=ArticleExt(id=1217845648460791964, articleId=1217845646913094647, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=超临界二氧化碳萃取法脱除绿茶中咖啡因工艺优化, columnId=1151895322281734685, journalTitle=食品安全质量检测学报, columnName=食品加工与工艺, runingTitle=null, highlight=null, articleAbstract=

目的 通过超临界二氧化碳萃取法探究绿茶中的咖啡因脱除工艺。方法 以婺源绿茶为原料, 通过超临界二氧化碳萃取法脱除绿茶中的咖啡因, 以咖啡因脱除率为考察指标, 采用单因素实验研究不同茶叶含水率, 萃取温度、压力、时间, 夹带剂浓度及用量对咖啡因脱除率的影响, 并通过正交实验优化咖啡因脱除工艺。结果 绿茶中咖啡因最佳脱除工艺为茶叶含水率40%, 萃取压力30 MPa, 萃取温度55 ℃, 萃取时间240 min, 夹带剂浓度为(乙醇)60%, 夹带剂用量选择1.2:1 (m:m), 此条件下的咖啡因脱除率为91.2%。萃取压力是影响咖啡因脱除率的最主要因素, 次之是萃取温度, 而萃取时间的影响相对最小。结论 本研究通过超临界二氧化碳萃取法确定了绿茶咖啡因最佳脱除工艺, 为脱除绿茶中的咖啡因提供了一定的参考。

, correspAuthors=刘晓华, authorNote=null, correspAuthorsNote=
* 刘晓华(1973—), 男, 博士, 研究员, 主要研究方向为食品生物技术。E-mail:
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许雯雯(1999—), 女, 硕士研究生, 主要研究方向为食品加工。E-mail:

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许雯雯(1999—), 女, 硕士研究生, 主要研究方向为食品加工。E-mail:

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许雯雯(1999—), 女, 硕士研究生, 主要研究方向为食品加工。E-mail:

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Journal of Food Science, 2009, 34(9): 206-210., articleTitle=Optimization of decaffeination process of green tea by supercritical CO2 using response surface method, refAbstract=null)], funds=[Fund(id=1217864256943477104, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, awardId=抚财文指〔2021〕43号, language=CN, fundingSource=抚州市重点研发计划项目(抚财文指〔2021〕43号), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1217864251583157244, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, xref=1, ext=[AuthorCompanyExt(id=1217864251591545853, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, companyId=1217864251583157244, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 Sino German Joint Research Institute, Nanchang University, Nanchang 330047, China), AuthorCompanyExt(id=1217864251599934462, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, companyId=1217864251583157244, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 南昌大学中德联合研究院, 南昌 330047)]), AuthorCompany(id=1217864251734151177, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, xref=2, ext=[AuthorCompanyExt(id=1217864251742539786, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, companyId=1217864251734151177, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 Jiangxi Provincial Key Laboratory of Agrofood Safety and Quality, Nanchang 330047, China), AuthorCompanyExt(id=1217864251746734091, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, companyId=1217864251734151177, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 农产品质量安全江西省重点实验室, 南昌 330047)])], figs=[ArticleFig(id=1217864256008147246, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, language=EN, label=Fig.1, caption=Effects of various factors on caffeine removal efficiency of green tea, figureFileSmall=mt4c/yHKjkVEVefjv3Bx2w==, figureFileBig=wwH/PNcl8F39yLLqE4b1rA==, tableContent=null), ArticleFig(id=1217864256121393462, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, language=CN, label=图1, caption=各因素对绿茶咖啡因脱除效率的影响

注: 不同小写字母表示差异显著(P<0.05)。

, figureFileSmall=mt4c/yHKjkVEVefjv3Bx2w==, figureFileBig=wwH/PNcl8F39yLLqE4b1rA==, tableContent=null), ArticleFig(id=1217864256289165635, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, language=EN, label=Table 1, caption=

Factor level table of orthogonal experimental

, figureFileSmall=null, figureFileBig=null, tableContent=
水平 因素
A(萃取压力)
/MPa		 B(萃取温度)
/℃		 C(萃取时间)
/min
1 25 50 180
2 30 55 210
3 35 60 240
), ArticleFig(id=1217864256398217546, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, language=CN, label=表1, caption=

正交实验因素水平表

, figureFileSmall=null, figureFileBig=null, tableContent=
水平 因素
A(萃取压力)
/MPa		 B(萃取温度)
/℃		 C(萃取时间)
/min
1 25 50 180
2 30 55 210
3 35 60 240
), ArticleFig(id=1217864256498880847, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, language=EN, label=Table 2, caption=

Results of orthogonal experimental

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实验号 A/MPa B/℃ C/min 咖啡因脱除率/%
1 1 1 1 70.1±4.2
2 1 2 2 75.5±4.3
3 1 3 3 80.2±3.9
4 2 1 2 78.1±4.0
5 2 2 3 91.2±5.1
6 2 3 1 85.9±4.3
7 3 1 3 83.5±3.7
8 3 2 1 86.3±4.1
9 3 3 2 90.5±5.0
k1 75.3 77.2 80.8
k2 85.1 84.3 81.3
k3 86.8 85.5 85.0
R 11.5 8.3 4.2
), ArticleFig(id=1217864256599544153, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1217845646913094647, language=CN, label=表2, caption=

正交实验结果

, figureFileSmall=null, figureFileBig=null, tableContent=
实验号 A/MPa B/℃ C/min 咖啡因脱除率/%
1 1 1 1 70.1±4.2
2 1 2 2 75.5±4.3
3 1 3 3 80.2±3.9
4 2 1 2 78.1±4.0
5 2 2 3 91.2±5.1
6 2 3 1 85.9±4.3
7 3 1 3 83.5±3.7
8 3 2 1 86.3±4.1
9 3 3 2 90.5±5.0
k1 75.3 77.2 80.8
k2 85.1 84.3 81.3
k3 86.8 85.5 85.0
R 11.5 8.3 4.2
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超临界二氧化碳萃取法脱除绿茶中咖啡因工艺优化
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许雯雯 1 , 戚琳悦 1 , 许辉良 1 , 刘晓华 1, 2, *
食品安全质量检测学报 | 食品加工与工艺 2025,16(16): 297-303
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食品安全质量检测学报 | 食品加工与工艺 2025, 16(16): 297-303
超临界二氧化碳萃取法脱除绿茶中咖啡因工艺优化
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许雯雯1 , 戚琳悦1, 许辉良1, 刘晓华1, 2, *
作者信息
  • 1 南昌大学中德联合研究院, 南昌 330047
  • 2 农产品质量安全江西省重点实验室, 南昌 330047

    • 许雯雯(1999—), 女, 硕士研究生, 主要研究方向为食品加工。E-mail:

通讯作者:

* 刘晓华(1973—), 男, 博士, 研究员, 主要研究方向为食品生物技术。E-mail:
Optimization of caffeine removal process in green tea by supercritical carbon dioxide extraction
Wen-Wen XU1 , Lin-Yue QI1, Hui-Liang XU1, Xiao-Hua LIU1, 2, *
Affiliations
  • 1 Sino German Joint Research Institute, Nanchang University, Nanchang 330047, China
  • 2 Jiangxi Provincial Key Laboratory of Agrofood Safety and Quality, Nanchang 330047, China
出版时间: 2025-08-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20250319001
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摘要
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目的 通过超临界二氧化碳萃取法探究绿茶中的咖啡因脱除工艺。方法 以婺源绿茶为原料, 通过超临界二氧化碳萃取法脱除绿茶中的咖啡因, 以咖啡因脱除率为考察指标, 采用单因素实验研究不同茶叶含水率, 萃取温度、压力、时间, 夹带剂浓度及用量对咖啡因脱除率的影响, 并通过正交实验优化咖啡因脱除工艺。结果 绿茶中咖啡因最佳脱除工艺为茶叶含水率40%, 萃取压力30 MPa, 萃取温度55 ℃, 萃取时间240 min, 夹带剂浓度为(乙醇)60%, 夹带剂用量选择1.2:1 (m:m), 此条件下的咖啡因脱除率为91.2%。萃取压力是影响咖啡因脱除率的最主要因素, 次之是萃取温度, 而萃取时间的影响相对最小。结论 本研究通过超临界二氧化碳萃取法确定了绿茶咖啡因最佳脱除工艺, 为脱除绿茶中的咖啡因提供了一定的参考。

婺源绿茶  /  超临界二氧化碳萃取法  /  咖啡因  /  脱除  /  正交实验

Objective To explore the process of caffeine removal from green tea by supercritical carbon dioxide extraction. Methods Using Wuyuan green tea as raw material, supercritical carbon dioxide extraction was used to remove caffeine from green tea. Taking the caffeine removal rate as the investigation index, the effects of tea moisture content, extraction temperature, pressure, time, concentration and dosage of entrained agent on caffeine removal rate were studied by single factor experiment, and the caffeine removal process was optimized by orthogonal experiment. Results The optimal extraction process of caffeine removal in green tea was tea moisture content 40%, extraction pressure 30 MPa, extraction temperature 55 ℃, extraction time 240 min, concentration of entrainment agent (ethanol) 60%, and dosage of entrainment agent 1.2:1 (m:m). Under these conditions, the caffeine removal rate was 91.2%. Extraction pressure was the most important factor affecting caffeine removal rate, followed by extraction temperature, and extraction time had relatively little effect. Conclusion This study determines the best technology of caffeine removal in green tea by supercritical carbon dioxide extraction, which provides a certain reference for caffeine removal in green tea.

Wuyuan green tea  /  supercritical carbon dioxide extraction  /  caffeine  /  removal  /  orthogonal experiment
许雯雯, 戚琳悦, 许辉良, 刘晓华. 超临界二氧化碳萃取法脱除绿茶中咖啡因工艺优化. 食品安全质量检测学报, 2025 , 16 (16) : 297 -303 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250319001
Wen-Wen XU, Lin-Yue QI, Hui-Liang XU, Xiao-Hua LIU. Optimization of caffeine removal process in green tea by supercritical carbon dioxide extraction[J]. Journal of Food Safety & Quality, 2025 , 16 (16) : 297 -303 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20250319001
正文
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0 引言
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茶作为全球消费量最大的饮品, 不仅具有保健功能, 且其独特的香气与风味也备受人们青睐。从发酵程度来看, 可以将茶分为3类, 未发酵茶、部分发酵茶与完全发酵茶。其中, 绿茶属于未发酵茶, 未发酵茶可以尽量避免在加工过程中发酵带来的如茶多酚、茶氨酸、茶多糖、维生素、矿物质和茶色素等功能性成分的损失, 具有调节肠道代谢和缓解肠道菌群失调、抗氧化、抗炎、预防血栓等功效[1-6]。咖啡因是茶叶中的重要活性成分, 其含量通常在1%~5%之间。大量研究显示, 心血管疾病患者、糖尿病患者、消化疾病患者、骨质疏松症患者、老年人、妊娠和哺乳期女性、青少年皆不宜长期饮用高咖啡因含量的茶叶[7-10], 因而脱咖啡因茶的需求量和消费量正在快速增长。另外, 被脱除的咖啡因也具有一定的药用价值, 如提神醒脑、利尿、消除水肿、刺激中枢神经系统和促进代谢等作用[11-12], 在医药、食品、运动营养、化妆品等领域得以广泛应用。由此可见, 脱咖啡因茶具有极大的市场潜力, 经济收益将十分可观。
目前常用的传统脱咖啡因茶的方法有: 有机溶剂法和热水浸提法[13]。有机溶剂法会在加工过程中使用二氯甲烷、氯仿和乙酸乙酯等有机化学溶剂, 且难以除净, 从而对人体造成伤害[14]。热水浸提法操作方便、工艺简单, 但咖啡因脱除率较低, 且在浸提过程中会掺杂一些易溶于水的成分, 如茶多酚、茶多糖等[15-16]。因此, 开发新的咖啡因脱除工艺在产业革新中至关重要。超临界二氧化碳萃取法是目前应用十分广泛的一种新型分离技术, 以提取效率高、有机物选择性强、溶解性能良好, 操作条件温和、安全无毒著称[17-18]。该方法选择性高, 能充分保留茶叶中的茶多酚、氨基酸等营养成分, 确保了茶叶的品质。在整个生产过程中, 二氧化碳被循环利用, 实现了零废水排放和零有毒气体释放, 确保了安全性和环保性[15]。超临界二氧化碳萃取技术对咖啡因的选择性较高, 可通过调节压力、温度和夹带剂显著提高脱除率, 并能结合动态循环萃取和在线分离技术, 缩短处理时间。该技术由于低热敏性能够尽可能保留茶叶的营养成分。近些年该技术也迎来革新, 如使用食品级夹带剂(如乳酸乙酯)替代传统乙醇, 极大地降低了残留的毒性。闭环系统设计可实现二氧化碳循环使用, 降低成本和环境负荷。但当前超临界二氧化碳脱除茶叶咖啡因技术仍面临若干关键性技术挑战: 在工艺经济性方面, 存在设备投资成本和能耗较大等规模化瓶颈; 在选择性控制方面, 需解决非咖啡因物质的共提取问题和夹带剂残留风险; 针对不同茶叶品种的基质差异, 需开发定制化工艺并实现水分的精准调控; 此外, 脱咖啡因茶叶的长期品质稳定性评估和标准化感官评价体系尚未完善; 最后, 新型夹带剂的安全认证和工业化规模下的高压系统安全保障等法规与工程问题也亟待解决。由于超临界二氧化碳脱除茶叶中咖啡因仍处于实验室研究阶段, 本研究拟通过工艺优化研究将超临界二氧化碳用于整叶绿茶的脱咖啡因生产, 以期为脱咖啡因茶产业开发和应用提供一定参考。
1 材料与方法
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1.1 材料与试剂
绿茶, 采购于江西省婺源县。
乙腈、二甲基甲酰胺(色谱纯, 西陇科学股份有限公司); 乙醇(分析纯, 北京索莱宝科技有限公司)。
1.2 仪器与设备
1200液相色谱仪[安捷伦科技(中国)有限公司]; Kromasil ODS色谱柱(250 mm×4.6 mm, 5 μm, 上海希言科学仪器有限公司); HA120-50-01超临界萃取装置(南通市华安超临界萃取有限公司); ME204分析天平(精度0.0001 g, 瑞士梅特勒-托利多公司)。
1.3 实验方法
1.3.1 咖啡因的萃取
将定量茶叶样品与乙醇夹带剂装入萃取釜, 调节至设定温度、压力后, 用超临界二氧化碳预浸30 min, 随后在设定分离条件下动态萃取, 收集产物并称重记录。
1.3.2 茶叶水分含量测定
按GB/T 8304—2013《茶 水分测定》的方法测定, 即将茶叶置于105 ℃烘箱中烘至恒重, 根据失重计算水分含量, 如式(1)所示。
水分含量/%=$\frac{{{m}_{1}}-{{m}_{2}}}{{{m}_{0}}}$×100%
式中: m1为试样和烘皿烘前的质量, g; m2为试样和烘皿烘后的质量, g; m0为试样的质量, g。
1.3.3 茶叶咖啡因含量的测定
按GB/T 8312—2013《茶 咖啡碱测定》的方法, 用高效液相色谱(high performance liquid chromatography, HPLC)法检测咖啡因的含量。
取萃取后的咖啡因用纯净水稀释到一定倍数, 取一部分试液, 通过0.45 μm滤膜过滤, 准确吸取过滤液10~20 μL, 注入HPLC, 并用咖啡碱系列标准工作液制作标准曲线, 进行色谱测定。咖啡碱含量计算公式如式(2)所示。
咖啡碱含量/%=$\frac{{{C}_{1}}\times {{V}_{1}}}{m\times w\times {{10}^{6}}}$×100%
式中: C1为根据标准曲线上计算得出的测定液中咖啡碱质量浓度, μg/mL; V1为样品总体积, mL; m为试样的质量, g; w为试样干物质含量(质量分数), %。
1.3.4 超临界萃取条件的单因素实验
根据1.3.1的实验方法, 以咖啡因脱除率为指标, 测定茶叶含水率(10%、20%、30%、40%、50%)、萃取压力(15、20、25、30、35 MPa)、萃取时间(30、90、150、210、270 min)、萃取温度(35、45、55、65、75 ℃)、夹带剂浓度(40%、50%、60%、70%和80%)和夹带剂用量(0.8:1、1.0:1、1.2:1、1.4:1和1.6:1) (m:m, 下同)对茶叶中咖啡因脱除的影响。各因素固定水平值: 茶叶含水量为30%, 萃取压力为25 MPa, 萃取温度为45 ℃, 萃取时间为150 min, 夹带剂浓度为60%, 夹带剂用量为1.0:1。
1.3.5 超临界萃取条件的正交实验
为了确定实验的最佳工艺条件, 在单因素实验的基础上, 进一步缩小实验因素范围, 采用4因素3水平正交表L9(34)进行正交实验, 探究萃取温度、萃取时间和萃取压力对咖啡因脱除率的影响。正交实验的因素水平表见表1。
1.4 数据处理
实验数据为3次重复实验的平均值, 采用平均值±标准偏差的形式表示。通过统计分析软件SPSS 19.0采用单因素方差法对数据进行单因素方差分析(P<0.01)和正交实验显著性分析(P<0.05), 采用Microsoft Excel 2021制表、绘图。
2 结果与分析
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2.1 茶叶含水率对绿茶咖啡因脱除效率的影响
相同条件下分别制备含水率为10%、20%、30%、40%和50%的茶叶样品, 通过超临界二氧化碳萃取法脱除茶叶中的咖啡因, 脱除结果如图1A所示。结果表明, 茶叶含水率对咖啡因脱除效率具有显著影响, 呈现先升高后降低的变化趋势。当含水率为10%的茶叶咖啡因脱除率仅达15.4%, 可能是由于咖啡因大部分以结合态存在, 较强的束缚力使咖啡因在超临界二氧化碳流体中溶解性较小[19], 故脱除率较低; 随着含水率的增加, 咖啡因脱除率也显著提高, 一方面由于茶叶水分含量增加, 茶叶对咖啡因的束缚力减小, 导致咖啡因游离出来[19]; 另一方面, 水分子使茶叶细胞膜肿胀, 加速咖啡因扩散[20-21]。此外, 部分咖啡因与二氧化碳互溶, 水分子起到一定的夹带剂作用[22]。当茶叶的含水率为40%时, 咖啡因脱除率达到最大, 为85.6%(图1A)。但随着含水率的持续增加, 咖啡因的脱除率开始下降, 这可能是由于咖啡因倾向于在过量的水相中保持可溶性, 并且水分含量较高时, 会在茶叶表面形成一层保护膜, 既不利于咖啡因渗出, 也会阻碍二氧化碳进入, 使得咖啡因难以萃取[23]。较高水分也会使物料黏连, 不利于从反应釜中取出, 严重时还可能造成机器堵塞。与TELLO等[20]的研究结果一致, 在低水分含量(16.4 wt%)与较高水分含量(64 wt%)时, 咖啡因提取率较低, 在中等水分含量(32 wt%和48 wt%)时, 咖啡因提取率最佳。因此, 茶叶含水率最优为40%。
2.2 不同萃取压力对绿茶咖啡因脱除效率的影响
在15、20、25、30和35 MPa的萃取压力条件下对咖啡因进行脱除, 结果如图1B所示。随着萃取压力的增加, 咖啡因脱除率也呈上升趋势, 这是因为随着萃取压力的升高, 二氧化碳密度也随之增加, 使得咖啡因溶解度也提高, 故咖啡因脱除率也显著提高, 此研究与蒋雨桥等[24]的研究成果具有较高的一致性。过高的萃取压力可能导致设备超负荷运行, 从而影响其稳定性和使用寿命。因此, 在综合考虑设备性能、运行安全性和脱除效率的基础上, 最终将萃取压力确定为30 MPa, 咖啡因脱除率为86.2%。
2.3 不同萃取温度对绿茶咖啡因脱除效率的影响
萃取温度是影响咖啡因脱除率的重要参数之一。萃取温度对绿茶咖啡因脱除率的影响如图1C所示。可以看出, 随着萃取温度的升高, 咖啡因脱除率逐渐提高, 在65 ℃时达到最高点, 之后开始降低。这可以通过萃取温度对二氧化碳密度的影响来解释[25]。随着温度的升高, 加快了二氧化碳分子间热运动, 提高了二氧化碳的溶解度, 增加了二氧化碳与咖啡因的接触机会, 继而提高了脱除率; 随着温度的持续升高, 导致二氧化碳密度降低, 又降低了二氧化碳的溶解度, 脱除率下降。过高的温度会使茶叶色泽暗淡和营养成分降解, 影响茶叶品质[26], 因此, 最适萃取温度为55 ℃, 此时咖啡因脱除率为86.1%。
2.4 不同萃取时间对绿茶咖啡因脱除效率的影响
萃取时间对咖啡因脱除率的影响如图1D所示, 整体呈现先快速上升后趋于平缓的变化趋势。实验结果表明, 在30~270 min范围内, 咖啡因脱除率从25.6%持续上升至94.7%, 其中90~210 min期间上升速率最为显著; 这一变化规律主要源于: 在萃取初期(30~90 min), 由于茶叶中咖啡因含量充足, 脱除率呈现稳定上升趋势; 在中期(90~210 min), 咖啡因在超临界流体中的溶解度接近饱和, 脱除率增速达到最大; 而后期(210~270 min)由于咖啡因逐渐耗尽, 脱除率虽仍保持增长但增幅明显降低[27]。综合考虑萃取效率与物料损耗等因素, 确定210 min为最佳萃取时间, 此时咖啡因脱除率可达85.9%。
2.5 夹带剂浓度对绿茶咖啡因脱除效率的影响
选取合适的夹带剂对咖啡因的脱除影响较大, 加入夹带剂可以改善二氧化碳的极性和溶解性能[28-29]。对咖啡因而言, 乙醇无毒、易除净, 萃取能力强。因此, 选择乙醇作为超临界流体萃取法脱除咖啡因的夹带剂。乙醇浓度选取为40%、50%、60%、70%、80%。由图1E可知, 咖啡因脱除率随着乙醇浓度的提高呈现上升趋势, 到达最高脱除率, 对应乙醇浓度为70%后, 咖啡因脱除率才逐步下降(图1E), 同时当乙醇的浓度超过80%时, 茶叶易变黄。乙醇浓度为60%或70%时, 咖啡因脱除率分别为85.6%和90.0%并无显著差异, 因此, 乙醇浓度选取60%。
2.6 夹带剂用量对绿茶咖啡因脱除效率的影响
在茶叶含水率40%、萃取压力30 MPa、萃取时间210 min、萃取温度55 ℃, 乙醇浓度60%条件下, 夹带剂与茶叶的质量比选择为0.8:1、1.0:1、1.2:1、1.4:1、1.6:1进行下一步探究。实验发现, 咖啡因脱除率随着夹带剂用量的增加呈先增后减趋势, 当夹带剂用量为1.2:1时, 咖啡因脱除率达到最大值86.2%(图1F), 但是夹带剂用量过多会导致液态萃取环境, 不利于进一步萃取[30-31]。姜爱莉等[32]的研究结果亦如此, 以乙酸乙酯为夹带剂, 随着乙酸乙酯用量的增加, 海鞘脂肪酸的得率并未增加反而下降。因此, 夹带剂用量选择1.2:1较为合适。
2.7 咖啡因脱除条件的正交实验
在单因素实验的基础上, 以咖啡因脱除率为主要指标, 选取对响应值有显著影响的因素进行正交实验, 即以咖啡因脱除率为指标, 根据前期单因素实验结果以及工厂实践表明, 萃取温度、萃取时间及萃取压力是影响实验效果的关键因素。以萃取压力(A)、萃取温度(B)、萃取时间(C)为考察因素, 根据1.3.5方法进行正交实验, 实验结果见表2。
正交实验结果和极差分析表明, 萃取压力对咖啡因脱除率影响最大, 其次为萃取温度, 萃取时间的影响最小。对正交实验结果进行的方差分析显示, 萃取压力对实验结果具有显著影响(P<0.05)。最佳的组合条件为A3B3C3, 即萃取压力为35 MPa、萃取温度为60 ℃、萃取时间240 min。在此条件下可以得到咖啡因脱除率为95.1%。
茶叶含水率是超临界萃取工艺中不可忽视的重要参数。朱尚彬等[33]在萃取温度为60 ℃、萃取压力为22 MPa, 50%乙醇萃取180 min的萃取条件下, 发现庐山毛尖的咖啡因脱除率仅为2.48%, 推测这与市售茶叶含水率(小于7%)过低有关, 含水率较低, 极大程度上影响了超临界流体的萃取, 可见含水率在萃取过程中起到的关键性作用。乙醇凭借其绿色环保特性与高效共溶能力, 在天然产物萃取领域被公认为理想型夹带剂。陈晓珍[34]采用60 ℃、28 MPa、210 min、加水量为20%的条件得到咖啡因脱除率为77.9%的脱咖啡因绿茶, 其中水起到了夹带剂的作用, 增加咖啡因在二氧化碳流体中的溶解度, 对比显示, 本研究采用乙醇作为夹带剂, 提取率显著提高。PARK等[35]在每100 g二氧化碳加入3.0 g、95% (V:V)乙醇夹带剂, 23 MPa, 63 ℃, 10 min内可以在10 g绿茶中提取96.60%的咖啡因, 虽然夹带剂含量高可以大大提高咖啡因脱除率, 但是有研究显示, 夹带剂添加过多, 会产生令人接受度低、不良气味“酒精味”, 这表明咖啡因脱除过程中可能残留一些夹带剂[36], 故需精准控制夹带剂用量。此外, 研究中还提到了在提取过程中会带出大量的叶绿素和儿茶素, 叶绿素的提取率会随着温度的提高而增大, 儿茶素也极易受到氧化、高温、光照和碱性环境的影响, 提取时间过长从而会影响茶叶的外观、香气和味道, 所以, 提取时间不宜太长。工艺参数的协同优化至关重要, 叶春林等[37]采用25 MPa, 50 ℃, 360 min, 含水率45%的萃取条件, 虽获得65.8%脱除率, 但长达6 h的萃取会导致茶叶中的营养成分大量损失。特别需关注萃取压力对活性成分的影响, 有相关研究, 在35 MPa的较高压力下进行超临界二氧化碳萃取时, 提取物中的多酚、类黄酮和抗氧化剂含量显著降低。综合考虑, 本研究选取含水率为40%, 萃取压力为30 MPa, 萃取温度55 ℃, 萃取时间为240 min, 夹带剂乙醇浓度为60%, 乙醇用量为1.2:1, 在此条件下咖啡因脱除率为91.2%, 可以最大程度上得到营养损失少, 咖啡因脱除率高的脱咖啡因茶。
3 结论
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综合考虑, 将实验条件选择为含水率40%, 萃取压力30 MPa, 萃取温度55 ℃, 萃取时间240 min, 夹带剂乙醇浓度为60%, 乙醇用量为1.2:1, 获得的咖啡因脱除率为91.2%。用超临界二氧化碳萃取法代替传统的咖啡因脱除工艺, 提高了咖啡因脱除率, 减少了营养物质的损失, 加工条件温和、加工过程安全无毒。脱咖啡因绿茶解决了因咖啡因而不能饮用绿茶的特定人群的问题, 得以让绿茶被广泛接受, 还为茶叶脱咖啡因工艺提供了重要的参考和指导。
基金
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  • 抚州市重点研发计划项目(抚财文指〔2021〕43号)
文献
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20250319001
  • 接收时间：2025-03-19
  • 首发时间：2026-01-13
  • 出版时间：2025-08-25
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  • 收稿日期：2025-03-19
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抚州市重点研发计划项目(抚财文指〔2021〕43号)
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    1 南昌大学中德联合研究院, 南昌 330047
    2 农产品质量安全江西省重点实验室, 南昌 330047

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* 刘晓华(1973—), 男, 博士, 研究员, 主要研究方向为食品生物技术。E-mail:
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2种不同金属材料的力学参数
科
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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