Article(id=1320883832102957234, tenantId=1146029695717560320, journalId=1260987677001138203, issueId=1320881884691808691, articleNumber=null, orderNo=null, doi=10.13386/j.issn1002-0306.2025080245, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1756051200000, receivedDateStr=2025-08-25, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1792852846407, onlineDateStr=2026-10-24, pubDate=1782835200000, pubDateStr=2026-07-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792852846407, onlineIssueDateStr=2026-10-24, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792852846407, creator=13701087609, updateTime=1792852846407, updator=13701087609, issue=Issue{id=1320881884691808691, tenantId=1146029695717560320, journalId=1260987677001138203, year='2026', volume='47', issue='13', pageStart='1', pageEnd='522', issueExtLink='null', onlineDate='null', pubDate='1782835200000', pubDateStr='2026-07-01', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792852382109, creator='13701087609', updateTime=1792852382109, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=226, endPage=236, ext={EN=ArticleExt(id=1320883832291700915, articleId=1320883832102957234, tenantId=1146029695717560320, journalId=1260987677001138203, language=EN, title=Dry Fractionation Combined with Solvent-assisted Fractionation for Process Optimization and Saturated Fatty Acid Enrichment in High-melting-point Mutton Tallow Fractions, columnId=1261343843090313538, journalTitle=Science and Technology of Food Industry, columnName=Processing Technology, runingTitle=null, highlight=null, articleAbstract=

To develop high value-added mutton tallow products, high-melting-point fractions were prepared from Altay sheep rump fat using a dry fractionation process combined with solvent-assisted fractionation. Solid fat yield, melting point, peroxide value, and acid value were selected as evaluation indices. Single-factor experiments were conducted to investigate the effects of various parameters on the fractionation efficiency, followed by Box-Behnken response surface design. The Analytic Hierarchy Process-Criteria Importance Through Intercriteria Correlation (AHP-CRITIC) method was applied to assign subjective and objective weights to each evaluation index, with the comprehensive score used as the response value. Physicochemical properties and fatty acid composition of the fractionated products were analyzed. The optimal conditions were determined as an oil-to-solvent ratio of 1:2, crystallization temperature of 20  °C, cooling rate of 8  °C/h, and crystallization time of 12  h. Under these conditions, the solid fat yield reached 33.23%, melting point was 50.1  °C, peroxide value was 0.02 mg/g, acid value was 0.42  mg/g, and the comprehensive score was 93.88. The high-melting-point mutton tallow fraction exhibited peroxide value, acid value, saponification value, malondialdehyde content, and iodine value of 0.025  mg/g, 0.44  mg/g, 195.38  mg/g, 1.94  nmol/mL, and 42.42  g/100 g, respectively, which were significantly lower than those of the raw tallow and the solid fat obtained by dry fractionation at 28  °C (28S) (P<0.05). The saturated fatty acid content increased from 43.94% in raw tallow to 47.8% in 28S, and further to 63.21% in the solid fat obtained by the combined fractionation method at 20  °C (20S). These results indicate that the high-melting-point fraction exhibits markedly enhanced oxidative stability and melting point, thereby improving its potential as a specialty fat. Compared with raw tallow, the saturated fatty acid content increased by 19.27% (P<0.05), providing a reference for the rational development of high-melting-point mutton tallow fractions and the enrichment process of saturated fatty acids.

, authors=Keyang ZHANG, Jintao WANG, Junfei YU, Lingyan WU, Dailin SHEN, Yan ZHANG, Zequan XU, Xin MA, Zirong WANG*, authorsList=Keyang ZHANG, Jintao WANG, Junfei YU, Lingyan WU, Dailin SHEN, Yan ZHANG, Zequan XU, Xin MA, Zirong WANG, authorCompany=null, correspAuthors=Zirong WANG, 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=1320883834346909888, articleId=1320883832102957234, tenantId=1146029695717560320, journalId=1260987677001138203, language=CN, title=干法分提协同溶剂法分提高熔点羊油组分工艺优化及饱和脂肪酸的富集, columnId=1261343845481066826, journalTitle=食品工业科技, columnName=工艺技术, runingTitle=null, highlight=null, articleAbstract=

为开发高附加值的羊油产品,以阿勒泰羊臀脂为原料,采用干法分提协同溶剂法分提工艺得到高熔点羊油组分。以固脂得率、熔点、过氧化值、酸价为评价指标,通过单因素实验,考察各因素对高熔点羊油组分分提效果的影响;应用Box-Behnken响应面法设计试验,结合AHP-CRITIC法对各评价指标进行主客观赋权,以综合评分为响应值。并对分提产物的理化性质和脂肪酸组成进行分析。结果表明:最优条件为油与溶剂比例1:2、养晶温度20 ℃、降温速率8 ℃/h、养晶时间12 h,在此条件下分提所得固脂得率为33.23%、熔点为50.1 ℃、过氧化值为0.02 mg/g、酸价为0.42 mg/g、综合评分为93.88。分提后所得高熔点羊油组分的过氧化值、酸价、皂化值、丙二醛、碘值分别为:0.025 mg/g、0.44 mg/g、195.38 mg/g、1.94 nmol/mL、42.42 g/100 g,显著低于原脂和干法分提所得固脂(28S)(P<0.05);28S的饱和脂肪酸由原脂的43.94%升高到47.8%,干法分提协同溶剂法分提后所得固脂(20S)饱和脂肪酸为63.21%。综上,分提所得高熔点羊油组分氧化稳定性和熔点有明显提升,增强了高熔点羊油组分作为特种油脂的使用价值;相较于原脂饱和脂肪酸显著提高19.27%(P<0.05),这为高熔点羊油组分的合理开发以及饱和脂肪酸的富集工艺提供了参考。

, authors=张可洋, 王锦涛, 于俊飞, 吴玲艳, 申岱林, 张炎, 徐泽权, 马欣, 王子荣*, authorsList=张可洋, 王锦涛, 于俊飞, 吴玲艳, 申岱林, 张炎, 徐泽权, 马欣, 王子荣, authorCompany=null, correspAuthors=王子荣, authorNote=

张可洋(2000−),女,硕士研究生,研究方向:食品营养,E-mail:

, correspAuthorsNote=
王子荣(1963−),男,博士,教授,研究方向:食品营养与安全,E-mail:。
, copyrightStatement=版权所有 © 2026《食品工业科技》编辑部, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=rqqaZsDws5+1dyClrP+8yg==, magXml=GKNMZfw0duOxiwB6gvTkpg==, pdfUrl=null, pdf=5fLMLuF4bA0P4BPErdTnUw==, pdfFileSize=6088268, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=NUxF3pgeO+G8k7G+Sa6f9g==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=gT3DAdkEh9vGykDF16uAOw==, mapNumber=null, fund=null)}, authors=[Author(id=1320883836179820741, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=3335355771@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1320883836267901127, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, authorId=1320883836179820741, language=EN, stringName=Keyang ZHANG, firstName=Keyang, middleName=null, lastName=ZHANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=College of Food Science and Pharmacy, Xinjiang Agricultural University, Urumqi 830052, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1320883836330815688, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, authorId=1320883836179820741, language=CN, stringName=张可洋, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=新疆农业大学食品科学与药学学院,新疆乌鲁木齐 830052, bio={"content":"

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Molecules, 2013, 18(1): 1036−1052., articleTitle=null, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1320883836095934657, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, xref=null, ext=[AuthorCompanyExt(id=1320883836104323266, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, companyId=1320883836095934657, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=College of Food Science and Pharmacy, Xinjiang Agricultural University, Urumqi 830052, China), AuthorCompanyExt(id=1320883836112711875, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, companyId=1320883836095934657, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=新疆农业大学食品科学与药学学院,新疆乌鲁木齐 830052)])], figs=[ArticleFig(id=1320883841275900153, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Fig.1, caption=Effect of different extraction solvents on yield and melting point of high-melting-point solid fat, figureFileSmall=GCQAcmM33dVvY+luhEE6xg==, figureFileBig=NUxF3pgeO+G8k7G+Sa6f9g==, tableContent=null), ArticleFig(id=1320883841359786234, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=图1, caption=不同分提溶剂对高熔点固脂得率和熔点的影响

注:不同小写字母代表数值间存在显著性差异(P<0.05),图2~图5同。

, figureFileSmall=GCQAcmM33dVvY+luhEE6xg==, figureFileBig=NUxF3pgeO+G8k7G+Sa6f9g==, tableContent=null), ArticleFig(id=1320883841611444475, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Fig.2, caption=Effect of different oil and solvent ratio on high-melting-point solid fat, figureFileSmall=aUKBRg3A2T7ylWU6ogEdlg==, figureFileBig=SD0a6LG5VJOU3/RHYoZyeA==, tableContent=null), ArticleFig(id=1320883841682747644, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=图2, caption=不同油与溶剂比例对高熔点固脂的影响, figureFileSmall=aUKBRg3A2T7ylWU6ogEdlg==, figureFileBig=SD0a6LG5VJOU3/RHYoZyeA==, tableContent=null), ArticleFig(id=1320883841754050813, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Fig.3, caption=Effects of different crystal curing temperatures on high-melting-point solid fat, figureFileSmall=xkX14JYhofo5PsM7NYB2PA==, figureFileBig=Eao9J9otlkVaw6c/B9V/gQ==, tableContent=null), ArticleFig(id=1320883841837936894, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=图3, caption=不同养晶温度对高熔点固脂的影响, figureFileSmall=xkX14JYhofo5PsM7NYB2PA==, figureFileBig=Eao9J9otlkVaw6c/B9V/gQ==, tableContent=null), ArticleFig(id=1320883841913434367, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Fig.4, caption=Effects of different cooling rates on high-melting-point solid fat, figureFileSmall=+fRVGxDacISymkp3xgirew==, figureFileBig=OhCiAwJxN9NaBayQcj7W2Q==, tableContent=null), ArticleFig(id=1320883841980543232, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=图4, caption=不同降温速率对高熔点固脂的影响, figureFileSmall=+fRVGxDacISymkp3xgirew==, figureFileBig=OhCiAwJxN9NaBayQcj7W2Q==, tableContent=null), ArticleFig(id=1320883842051846401, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Fig.5, caption=Effects of different crystal cultivation times on high-melting-point solid fat, figureFileSmall=ua8fRfQNrze1oltNowDGXg==, figureFileBig=HwXPuh7joXgw9CK5ZQQLFg==, tableContent=null), ArticleFig(id=1320883842118955266, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=图5, caption=不同养晶时间对高熔点固脂的影响, figureFileSmall=ua8fRfQNrze1oltNowDGXg==, figureFileBig=HwXPuh7joXgw9CK5ZQQLFg==, tableContent=null), ArticleFig(id=1320883842186064131, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Fig.6, caption=Influence of different factors on the overall score, figureFileSmall=gsztYOBtnN5jsxHqW2vXtg==, figureFileBig=TZ5H9lkM4D9mBkyvKKETpw==, tableContent=null), ArticleFig(id=1320883842257367300, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=图6, caption=不同因素对综合评分的影响, figureFileSmall=gsztYOBtnN5jsxHqW2vXtg==, figureFileBig=TZ5H9lkM4D9mBkyvKKETpw==, tableContent=null), ArticleFig(id=1320883842311893253, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 1, caption=

Factors and levels of response surface experimental design

, figureFileSmall=null, figureFileBig=null, tableContent=
因素水平
−101
A:油与溶剂比例(v/v)1:11:21:3
B:养晶温度(℃)172023
C:降温速率(℃/h)6810
D:养晶时间(h)91215
), ArticleFig(id=1320883842374807814, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表1, caption=

响应面试验设计因素水平

, figureFileSmall=null, figureFileBig=null, tableContent=
因素水平
−101
A:油与溶剂比例(v/v)1:11:21:3
B:养晶温度(℃)172023
C:降温速率(℃/h)6810
D:养晶时间(h)91215
), ArticleFig(id=1320883842450305287, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 2, caption=

Evaluation index judgment matrix for high-melting-point solid fats

, figureFileSmall=null, figureFileBig=null, tableContent=
考察指标判断矩阵WiCR
熔点得率过氧化值酸价
熔点1.0002.0003.0003.0000.45470.004
得率0.5001.0002.0002.0000.2630
过氧化值0.3330.5001.0001.0000.1411
酸价0.3330.5001.0001.0000.1411
), ArticleFig(id=1320883842504831240, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表2, caption=

高熔点固脂评价指标判断矩阵

, figureFileSmall=null, figureFileBig=null, tableContent=
考察指标判断矩阵WiCR
熔点得率过氧化值酸价
熔点1.0002.0003.0003.0000.45470.004
得率0.5001.0002.0002.0000.2630
过氧化值0.3330.5001.0001.0000.1411
酸价0.3330.5001.0001.0000.1411
), ArticleFig(id=1320883842584523017, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 3, caption=

Composition of high-melting-point solid fat fatty acids under different extraction solvents

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸(%)28S丙酮20S丙酮15S异丙醇30S异丙醇25S
肉豆蔻酸2.87±0.00d3.13±0.01b3.32±0.02a2.92±0.03c2.90±0.02c
肉蔻油酸0.31±0.00a0.20±0.00d0.20±0.00d0.25±0.00c0.27±0.00b
十五(烷)酸1.48±0.00ab1.44±0.01d1.49±0.00a1.46±0.01cd1.47±0.01bc
棕榈酸23.36±0.03e27.86±0.19b28.25±0.03a25.98±0.17c24.60±0.15d
棕榈油酸2.79±0.00a2.19±0.01e2.23±0.00d2.45±0.02c2.62±0.02b
十七(烷)酸3.14±0.00e3.77±0.03b3.82±0.01a3.52±0.02c3.31±0.02d
硬脂酸16.95±0.02d27.01±0.25a26.77±0.10a22.76±0.09b19.62±0.11c
反-9-十八稀酸4.00±0.01a2.92±0.05c3.05±0.03bc3.22±0.53bc3.64±0.57ab
油酸36.56±0.00a25.37±0.16d25.05±0.03e30.44±0.16c33.80±0.23b
反亚油酸0.91±0.00a0.67±0.01d0.68±0.01d0.78±0.01c0.86±0.00b
亚油酸3.66±0.01a2.42±0.01d2.36±0.00e3.00±0.03c3.34±0.02b
亚麻酸1.38±0.00a0.91±0.00d0.88±0.00e1.13±0.01c1.28±0.01b
饱和47.80±0.01d63.21±0.49a63.64±0.12a56.63±0.32b51.90±0.31c
不饱和49.61±0.01a34.61±0.13d34.43±0.05d41.26±0.31c45.81±0.29b
), ArticleFig(id=1320883842664214794, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表3, caption=

不同分提溶剂下高熔点固脂脂肪酸组成

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸(%)28S丙酮20S丙酮15S异丙醇30S异丙醇25S
肉豆蔻酸2.87±0.00d3.13±0.01b3.32±0.02a2.92±0.03c2.90±0.02c
肉蔻油酸0.31±0.00a0.20±0.00d0.20±0.00d0.25±0.00c0.27±0.00b
十五(烷)酸1.48±0.00ab1.44±0.01d1.49±0.00a1.46±0.01cd1.47±0.01bc
棕榈酸23.36±0.03e27.86±0.19b28.25±0.03a25.98±0.17c24.60±0.15d
棕榈油酸2.79±0.00a2.19±0.01e2.23±0.00d2.45±0.02c2.62±0.02b
十七(烷)酸3.14±0.00e3.77±0.03b3.82±0.01a3.52±0.02c3.31±0.02d
硬脂酸16.95±0.02d27.01±0.25a26.77±0.10a22.76±0.09b19.62±0.11c
反-9-十八稀酸4.00±0.01a2.92±0.05c3.05±0.03bc3.22±0.53bc3.64±0.57ab
油酸36.56±0.00a25.37±0.16d25.05±0.03e30.44±0.16c33.80±0.23b
反亚油酸0.91±0.00a0.67±0.01d0.68±0.01d0.78±0.01c0.86±0.00b
亚油酸3.66±0.01a2.42±0.01d2.36±0.00e3.00±0.03c3.34±0.02b
亚麻酸1.38±0.00a0.91±0.00d0.88±0.00e1.13±0.01c1.28±0.01b
饱和47.80±0.01d63.21±0.49a63.64±0.12a56.63±0.32b51.90±0.31c
不饱和49.61±0.01a34.61±0.13d34.43±0.05d41.26±0.31c45.81±0.29b
), ArticleFig(id=1320883842785849611, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 4, caption=

Box-Behnken design and corresponding experimental results

, figureFileSmall=null, figureFileBig=null, tableContent=
试验号A:油与溶剂比例B:养晶温度(℃)C:降温
速率(℃/h)
D:养晶时间(h)Y:综合评分
11:11781277.80
21:31781274.90
31:12381276.34
41:32381268.88
51:2206979.97
61:22010975.81
71:22061579.58
81:220101577.11
91:1208976.51
101:3208969.29
111:12081575.90
121:32081571.32
131:21761282.82
141:22361275.50
151:217101278.59
161:223101276.97
171:12061276.73
181:32061272.90
191:120101277.79
201:320101269.75
211:2178978.45
221:2238974.16
231:21781580.47
241:22381575.84
251:22081293.08
261:22081293.04
271:22081293.59
281:22081293.36
291:22081295.98
), ArticleFig(id=1320883842878124300, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表4, caption=

响应面试验设计与结果

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试验号A:油与溶剂比例B:养晶温度(℃)C:降温
速率(℃/h)
D:养晶时间(h)Y:综合评分
11:11781277.80
21:31781274.90
31:12381276.34
41:32381268.88
51:2206979.97
61:22010975.81
71:22061579.58
81:220101577.11
91:1208976.51
101:3208969.29
111:12081575.90
121:32081571.32
131:21761282.82
141:22361275.50
151:217101278.59
161:223101276.97
171:12061276.73
181:32061272.90
191:120101277.79
201:320101269.75
211:2178978.45
221:2238974.16
231:21781580.47
241:22381575.84
251:22081293.08
261:22081293.04
271:22081293.59
281:22081293.36
291:22081295.98
), ArticleFig(id=1320883842970398989, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 5, caption=

Regression model analysis of variance

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方差来源平方和自由度均方差F值P值显著性
模型1598.7914114.2131.14<0.0001**
A96.46196.46110.78<0.0001**
B53.56153.5661.5<0.0001**
C10.96110.9612.590.0032**
D3.0213.023.470.0837
AB5.1915.195.970.0285*
AC4.4414.445.10.0404*
AD1.7511.752.010.1783
BC8.1318.139.330.0086**
BD0.028110.02810.03230.8599
CD0.715210.71520.82130.3801
A2913.091913.091048.56<0.0001**
B2393.771393.77452.19<0.0001**
C2359.011359.01412.28<0.0001**
D2477.311477.31548.12<0.0001**
残差12.19140.8708
失拟项6.1100.61010.40070.8902
纯误差6.0941.52
总离差1610.9828
), ArticleFig(id=1320883843033313550, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表5, caption=

回归模型方差分析

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方差来源平方和自由度均方差F值P值显著性
模型1598.7914114.2131.14<0.0001**
A96.46196.46110.78<0.0001**
B53.56153.5661.5<0.0001**
C10.96110.9612.590.0032**
D3.0213.023.470.0837
AB5.1915.195.970.0285*
AC4.4414.445.10.0404*
AD1.7511.752.010.1783
BC8.1318.139.330.0086**
BD0.028110.02810.03230.8599
CD0.715210.71520.82130.3801
A2913.091913.091048.56<0.0001**
B2393.771393.77452.19<0.0001**
C2359.011359.01412.28<0.0001**
D2477.311477.31548.12<0.0001**
残差12.19140.8708
失拟项6.1100.61010.40070.8902
纯误差6.0941.52
总离差1610.9828
), ArticleFig(id=1320883844677480719, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 6, caption=

Results of validation tests

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实验号固脂得率
(%)
固脂熔点
(℃)
过氧化值
(mg/g)
酸价
(mg/g)
综合评分
133.5049.40.0220.4294.08
232.8050.40.0230.4393.43
333.4050.50.0240.4094.13
平均值33.2350.10.0200.4293.88
), ArticleFig(id=1320883844765561104, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表6, caption=

验证实验结果

, figureFileSmall=null, figureFileBig=null, tableContent=
实验号固脂得率
(%)
固脂熔点
(℃)
过氧化值
(mg/g)
酸价
(mg/g)
综合评分
133.5049.40.0220.4294.08
232.8050.40.0230.4393.43
333.4050.50.0240.4094.13
平均值33.2350.10.0200.4293.88
), ArticleFig(id=1320883844841058577, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 7, caption=

Physicochemical indexes of sheep buttock fat before and after fractionation

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理化指标原脂(分提前)28℃固脂(28S)分提后固脂(20S)
水分(%)0.47±0.03a0.22±0.02b0.22±0.01b
过氧化值(mg/g)0.06±0.002a0.048±0.003b0.025±0.003c
酸价(mg/g)0.7±0.05a0.54±0.04b0.44±0.03c
碘值(g/100 g)52.19±1.96a46.72±1.37b42.42±1.99c
皂化值(mg/g)202.03±1.55a197.65±0.88b195.38±1.55c
丙二醛(nmol/mL)2.49±0.10a2.18±0.12b1.94±0.12c
), ArticleFig(id=1320883844912361746, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表7, caption=

分提前后羊臀脂的理化指标

, figureFileSmall=null, figureFileBig=null, tableContent=
理化指标原脂(分提前)28℃固脂(28S)分提后固脂(20S)
水分(%)0.47±0.03a0.22±0.02b0.22±0.01b
过氧化值(mg/g)0.06±0.002a0.048±0.003b0.025±0.003c
酸价(mg/g)0.7±0.05a0.54±0.04b0.44±0.03c
碘值(g/100 g)52.19±1.96a46.72±1.37b42.42±1.99c
皂化值(mg/g)202.03±1.55a197.65±0.88b195.38±1.55c
丙二醛(nmol/mL)2.49±0.10a2.18±0.12b1.94±0.12c
), ArticleFig(id=1320883844987859219, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=EN, label=Table 8, caption=

Fatty acid composition of sheep buttock fat before and after fractionation

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脂肪酸(%)原脂(分提前)28℃固脂(28S)分提后固脂(20S)
肉豆蔻酸2.73±0.01c2.87±0.00b3.13±0.01a
肉蔻油酸0.34±0.00a0.31±0.00b0.20±0.00c
十五(烷)酸1.47±0.01a1.48±0.00a1.44±0.01b
棕榈酸22.10±0.01c23.36±0.03b27.86±0.19a
棕榈油酸2.92±0.01a2.79±0.00b2.19±0.01c
十七(烷)酸2.97±0.01c3.14±0.00b3.77±0.03a
硬脂酸14.67±0.04c16.95±0.02b27.01±0.25a
反−9−十八稀酸4.00±0.01a4.00±0.01a2.92±0.05b
油酸39.55±0.00a36.56±0.00b25.37±0.16c
反亚油酸0.96±0.00a0.91±0.00b0.67±0.01c
亚油酸3.98±0.01a3.66±0.01b2.42±0.01c
亚麻酸1.50±0.01a1.38±0.00b0.91±0.00c
饱和43.94±0.02c47.80±0.01b63.21±0.49a
不饱和53.25±0.01a49.61±0.01b34.61±0.13c
), ArticleFig(id=1320883845050773780, tenantId=1146029695717560320, journalId=1260987677001138203, articleId=1320883832102957234, language=CN, label=表8, caption=

分提前后羊臀脂的脂肪酸组成

, figureFileSmall=null, figureFileBig=null, tableContent=
脂肪酸(%)原脂(分提前)28℃固脂(28S)分提后固脂(20S)
肉豆蔻酸2.73±0.01c2.87±0.00b3.13±0.01a
肉蔻油酸0.34±0.00a0.31±0.00b0.20±0.00c
十五(烷)酸1.47±0.01a1.48±0.00a1.44±0.01b
棕榈酸22.10±0.01c23.36±0.03b27.86±0.19a
棕榈油酸2.92±0.01a2.79±0.00b2.19±0.01c
十七(烷)酸2.97±0.01c3.14±0.00b3.77±0.03a
硬脂酸14.67±0.04c16.95±0.02b27.01±0.25a
反−9−十八稀酸4.00±0.01a4.00±0.01a2.92±0.05b
油酸39.55±0.00a36.56±0.00b25.37±0.16c
反亚油酸0.96±0.00a0.91±0.00b0.67±0.01c
亚油酸3.98±0.01a3.66±0.01b2.42±0.01c
亚麻酸1.50±0.01a1.38±0.00b0.91±0.00c
饱和43.94±0.02c47.80±0.01b63.21±0.49a
不饱和53.25±0.01a49.61±0.01b34.61±0.13c
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干法分提协同溶剂法分提高熔点羊油组分工艺优化及饱和脂肪酸的富集
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张可洋 , 王锦涛 , 于俊飞 , 吴玲艳 , 申岱林 , 张炎 , 徐泽权 , 马欣 , 王子荣 *
食品工业科技 | 工艺技术 2026,47(13): 226-236
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食品工业科技 |工艺技术 2026 , 47 (13) : 226 -236
干法分提协同溶剂法分提高熔点羊油组分工艺优化及饱和脂肪酸的富集
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张可洋 , 王锦涛, 于俊飞, 吴玲艳, 申岱林, 张炎, 徐泽权, 马欣, 王子荣*
作者信息
  • 新疆农业大学食品科学与药学学院,新疆乌鲁木齐 830052
通讯作者:
王子荣(1963−),男,博士,教授,研究方向:食品营养与安全,E-mail:。
作者简介:

张可洋(2000−),女,硕士研究生,研究方向:食品营养,E-mail:

Dry Fractionation Combined with Solvent-assisted Fractionation for Process Optimization and Saturated Fatty Acid Enrichment in High-melting-point Mutton Tallow Fractions
Keyang ZHANG , Jintao WANG, Junfei YU, Lingyan WU, Dailin SHEN, Yan ZHANG, Zequan XU, Xin MA, Zirong WANG*
Affiliations
  • College of Food Science and Pharmacy, Xinjiang Agricultural University, Urumqi 830052, China
出版时间: 2026-07-01 doi: 10.13386/j.issn1002-0306.2025080245
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为开发高附加值的羊油产品,以阿勒泰羊臀脂为原料,采用干法分提协同溶剂法分提工艺得到高熔点羊油组分。以固脂得率、熔点、过氧化值、酸价为评价指标,通过单因素实验,考察各因素对高熔点羊油组分分提效果的影响;应用Box-Behnken响应面法设计试验,结合AHP-CRITIC法对各评价指标进行主客观赋权,以综合评分为响应值。并对分提产物的理化性质和脂肪酸组成进行分析。结果表明:最优条件为油与溶剂比例1:2、养晶温度20 ℃、降温速率8 ℃/h、养晶时间12 h,在此条件下分提所得固脂得率为33.23%、熔点为50.1 ℃、过氧化值为0.02 mg/g、酸价为0.42 mg/g、综合评分为93.88。分提后所得高熔点羊油组分的过氧化值、酸价、皂化值、丙二醛、碘值分别为:0.025 mg/g、0.44 mg/g、195.38 mg/g、1.94 nmol/mL、42.42 g/100 g,显著低于原脂和干法分提所得固脂(28S)(P<0.05);28S的饱和脂肪酸由原脂的43.94%升高到47.8%,干法分提协同溶剂法分提后所得固脂(20S)饱和脂肪酸为63.21%。综上,分提所得高熔点羊油组分氧化稳定性和熔点有明显提升,增强了高熔点羊油组分作为特种油脂的使用价值;相较于原脂饱和脂肪酸显著提高19.27%(P<0.05),这为高熔点羊油组分的合理开发以及饱和脂肪酸的富集工艺提供了参考。

羊臀脂  /  干法分提协同溶剂法分提  /  高熔点羊油组分  /  饱和脂肪酸

To develop high value-added mutton tallow products, high-melting-point fractions were prepared from Altay sheep rump fat using a dry fractionation process combined with solvent-assisted fractionation. Solid fat yield, melting point, peroxide value, and acid value were selected as evaluation indices. Single-factor experiments were conducted to investigate the effects of various parameters on the fractionation efficiency, followed by Box-Behnken response surface design. The Analytic Hierarchy Process-Criteria Importance Through Intercriteria Correlation (AHP-CRITIC) method was applied to assign subjective and objective weights to each evaluation index, with the comprehensive score used as the response value. Physicochemical properties and fatty acid composition of the fractionated products were analyzed. The optimal conditions were determined as an oil-to-solvent ratio of 1:2, crystallization temperature of 20  °C, cooling rate of 8  °C/h, and crystallization time of 12  h. Under these conditions, the solid fat yield reached 33.23%, melting point was 50.1  °C, peroxide value was 0.02 mg/g, acid value was 0.42  mg/g, and the comprehensive score was 93.88. The high-melting-point mutton tallow fraction exhibited peroxide value, acid value, saponification value, malondialdehyde content, and iodine value of 0.025  mg/g, 0.44  mg/g, 195.38  mg/g, 1.94  nmol/mL, and 42.42  g/100 g, respectively, which were significantly lower than those of the raw tallow and the solid fat obtained by dry fractionation at 28  °C (28S) (P<0.05). The saturated fatty acid content increased from 43.94% in raw tallow to 47.8% in 28S, and further to 63.21% in the solid fat obtained by the combined fractionation method at 20  °C (20S). These results indicate that the high-melting-point fraction exhibits markedly enhanced oxidative stability and melting point, thereby improving its potential as a specialty fat. Compared with raw tallow, the saturated fatty acid content increased by 19.27% (P<0.05), providing a reference for the rational development of high-melting-point mutton tallow fractions and the enrichment process of saturated fatty acids.

sheep rump fat  /  dry fractionation combined with solvent-assisted fractionation  /  high-melting-point mutton tallow fraction  /  saturated fatty acids
张可洋, 王锦涛, 于俊飞, 吴玲艳, 申岱林, 张炎, 徐泽权, 马欣, 王子荣. 干法分提协同溶剂法分提高熔点羊油组分工艺优化及饱和脂肪酸的富集. 食品工业科技, 2026 , 47 (13) : 226 -236 . DOI: 10.13386/j.issn1002-0306.2025080245
Keyang ZHANG, Jintao WANG, Junfei YU, Lingyan WU, Dailin SHEN, Yan ZHANG, Zequan XU, Xin MA, Zirong WANG. Dry Fractionation Combined with Solvent-assisted Fractionation for Process Optimization and Saturated Fatty Acid Enrichment in High-melting-point Mutton Tallow Fractions[J]. Science and Technology of Food Industry, 2026 , 47 (13) : 226 -236 . DOI: 10.13386/j.issn1002-0306.2025080245
羊油是一种优质食用油脂,含有丰富的营养成分和生物活性物质[1]。阿勒泰羊是新疆特色绵羊品种,其臀脂资源丰富,约占出栏体重的17%。阿勒泰羊臀脂兼具独特风味与优良加工性能,是极具开发价值的区域性动物油脂资源[2−4]。高熔点食用油脂如棕榈硬脂、猪油和牛油等在食品加工业具有广泛用途,如作为涂抹脂、起酥油、人造奶油和煎炸油等特种油脂[5]。其具备高烟点与优良的氧化稳定性,适合开发高温煎炸油[6−7];特定的高熔点油脂是制备优质起酥油与涂抹脂的理想原料[5]。因此,高效获取高纯度的高熔点油脂组分,对特种油脂的开发至关重要。羊油作为多种不同熔点甘油三酯的混合物,限制了其在食品加工中的应用,可通过分提技术获取特定熔点的功能性组分,以满足特种油脂的精准化生产需求[8]。
油脂干法分提操作简单、成本低,任航歧等[9]通过多级干法分提羊臀脂得到高熔点羊油组分,发现制作的起酥油面包的品质优于市售猪油基起酥油面包。溶剂法分提能提高分离效率,Salas等[10]通过溶剂分提将葵花籽油转化为高硬脂酸黄油,实现了对可可脂的有效替代。但单一的干法分提固液分离效率低,限制了其在高纯度产品制备中的应用[11];单一的溶剂法分提对高熔点羊油组分的选择性不足[12]。因此迫切需要开发一种高效的分提工艺,用于制备高纯度高熔点羊油组分,本研究提出将干法与溶剂法分提相协同的新工艺,其核心创新在于通过过程耦合与参数优化,同步提升高熔点羊油组分的分提效率与纯度。
本研究以阿勒泰羊臀脂为原料,采用干法分提协同溶剂法分提高熔点羊油组分,通过控制分提过程中的油与溶剂比例、养晶温度、降温速率、养晶时间,利用单因素实验和响应面法优化分提工艺,并对分提产物的理化性质和脂肪酸组成进行分析,研究该工艺对羊油理化性质和脂肪酸组成的影响,为富集饱和脂肪酸拓宽思路,以期突破现有分提技术瓶颈并为高熔点羊油组分的高效制备及特种油脂的开发和利用提供理论依据和技术支持。
阿勒泰羊臀脂(15月龄雄性) 新疆乌鲁木齐华凌牛羊屠宰场;硫代硫酸钠、韦氏(Wijs)试剂、37种脂肪酸甲酯混合标准品 上海源叶生物科技有限公司;丙二醛ELISA试剂盒 苏州梦犀生物医药科技有限公司;可溶性淀粉(食品级) 上海麦克林生化科技股份有限公司;氢氧化钾、甲醇、丙酮、异丙醇、正己烷、石油醚(60~90)、三氯甲烷、冰乙酸、碘化钾、乙醚、氢氧化钠、无水乙醇、环己烷、盐酸等 均为分析纯。
Al 204-IC型电子分析天平 梅特勒-托利多仪器(上海)有限公司;HHS(数显式)型电热恒温水浴锅 北京科伟永兴仪器有限公司;SPX-150型生化培养箱 深圳市三诺仪器仪表经营部;4-20R型冷冻离心机 江苏恒诺仪器制造有限公司;TG 16-WS型高速台式离心机 湖南湘仪实验室仪器开发有限公司;FL-1型可调式封闭电炉 北京市永光明医疗器械有限公司;DZF型真空干燥箱 恒诺利兴科技有限公司;DHS-16型水分测定仪 上海菁海仪器有限公司;Agilent 7890B型气相色谱仪 安捷伦科技有限公司。
采用王锦涛等[13]的方法进行制备,羊臀脂去除结缔组织,分割成约5 cm×5 cm×5 cm的小块放入绞肉机绞碎,绞碎后,准确称取100 g后放入烧杯并用电炉加热,采用干法熬制熔化羊臀脂至不再出油为止,随后用纱布过滤油渣得到粗提羊油,收集液体部分于−25 ℃密封保存。
称取适量的粗提羊油分装至50 mL的离心管中,将其放置水浴锅内加热至60 ℃,完全熔化后,置于培养箱内加热至平衡温度60 ℃并保持30 min以消除结晶记忆,以8 ℃/h的降温速率梯度降温至28 ℃,在此温度下养晶9 h后使用冷冻离心机在4000 r/min条件下离心15 min得到固脂和液油,将28 ℃条件下分提所得固脂(28S)加热至60 ℃完全熔化后,添加溶剂,充分摇匀,置于培养箱内加热至平衡温度40 ℃保持30 min以消除结晶记忆,按一定速率降温至养晶温度,养晶一段时间后分离固脂与液油,在70 ℃、0.08 MPa条件下真空干燥4 h以去除油脂中的溶剂残留,密封后−25 ℃冻藏备用。
根据不同溶剂(异丙醇、丙酮、正己烷、石油醚)的结晶温度,设定养晶温度(异丙醇30 ℃、丙酮20 ℃、正己烷15 ℃、石油醚15 ℃)。在8 ℃/h的降温速率、9 h的养晶时间、油与溶剂比例1:2的条件下,考察四种分提溶剂对高熔点固脂的得率、熔点的影响,筛选出异丙醇、丙酮两种分提溶剂;继续降低养晶温度(异丙醇25 ℃、丙酮15 ℃),在同一条件下,考察分提溶剂对高熔点固脂脂肪酸的影响,筛选出最合适的溶剂进行单因素实验。
以分提产物高熔点固脂的得率、熔点、过氧化值、酸价为评价指标,选择油与溶剂比例、养晶温度、降温速率、养晶时间进行单因素实验。
在丙酮作为分提溶剂,养晶温度20 ℃,降温速率8 ℃/h,养晶时间9 h的条件下,考察不同油与溶剂比例(v/v)(1:1、1:2、1:3、1:4、1:5)对固脂的得率、熔点、过氧化值、酸价的影响。
在丙酮作为分提溶剂,油与溶剂比例1:2,降温速率8 ℃/h,养晶时间9 h的条件下,考察不同养晶温度(23、20、17、14、11 ℃)对固脂的得率、熔点、过氧化值、酸价的影响。
在丙酮作为分提溶剂,油与溶剂比例1:2,养晶温度20 ℃,养晶时间9 h的条件下,考察不同降温速率(4、6、8、10、12 ℃/h)对固脂的得率、熔点、过氧化值、酸价的影响。
在丙酮作为分提溶剂,油与溶剂比例1:2,养晶温度20 ℃,降温速率8 ℃/h的条件下,考察不同养晶时间(3、6、9、12、15 h)对固脂的得率、熔点、过氧化值、酸价的影响。
在单因素实验的基础上,选取油与溶剂比例(A)、养晶温度(B)、降温速率(C)、养晶时间(D)为自变量,以高熔点固脂各评价指标(固脂的得率、熔点、过氧化值、酸价)的综合评分为响应值,导入Design-Expert 13软件进行四因素三水平共29个试验点的响应面试验设计,各因素水平表见表1。
根据相关研究[14−16],将固脂得率、熔点、过氧化值、酸价4个评价指标按照重要程度分为4个层次,构造判断矩阵,并进行一致性检验,计算结果见表2,所得各评价指标的权重WAHPi依次为:固脂得率0.2630、固脂熔点0.4547、固脂过氧化值0.1411、固脂酸价0.1411,一致性比率CR为0.004<0.1,符合一致性检验要求。
根据相关研究[14−16],通过CRITIC法计算各评价指标客观权重系数,使用SPSS27.0对实验数据进行归一化处理,对归一化的数据进行CRITIC分析,计算所得各评价指标的权重WCRITICi依次为:固脂得率0.2397、固脂熔点0.2230、固脂过氧化值0.3014、固脂酸价0.2358。
AHP是主观赋权法,CRITIC法是客观赋权法,将AHP法和CRITIC法进行结合,相较于单一赋权法能够更科学合理地评估各指标的综合权重。因此选择AHP-CRITIC法按照公式(1)计算响应面试验中各指标的综合权重。综合权重系数WAHP-CRITIC分依次为:固脂得率0.2624、固脂熔点0.4220、固脂过氧化值0.1770、固脂酸价0.1385。
$ \rm {W}_{AHP-CRITIC}=\frac{{W}_{AHP}\times {W}_{CRITIC}}{\displaystyle\sum\nolimits_{j=1}^{n}{W}_{AHP\times CRITIC}} $
根据综合权重系数按照公式(2)和公式(3)计算评价指标的综合评分:Wj为第j个指标的综合权重系数;Fj为第j个评价指标的实验结果;(Fj)max为实验组中第j个指标的最大值;(Fj)min为实验组中第j个指标的最小值。其中固脂得率和固脂熔点两个评价指标的综合评分采用公式(2)进行计算为M1;固脂过氧化值和固脂酸价两个评价指标的综合评分采用公式(3)进行计算为M2,四个评价指标的综合评分为两次计算结果的加和,即M1+M2。
$ \rm M1=\displaystyle\sum\nolimits_{j=1}^{n}\frac{{W}_{j}\times {F}_{j}}{{({F}_{j})}_{\max }}\times 100 $
$ \rm M2=\displaystyle\sum\nolimits_{j=1}^{n}\frac{{W}_{j}\times {({F}_{j})}_{\min }}{{F}_{j}}\times 100 $
得率的计算公式如下:
$ \rm R({\text{%}})=\frac{m}{M}\times 100 $
式中:R为固脂得率(%);M为干法分提所得28S的重量(g);m为分提所得固脂的重量(g)。
熔点的测定参照GB/T 12766-2008《动物油脂熔点的测定》;过氧化值的测定参照GB 5009.227-2023 《食品安全国家标准 食品中过氧化值的测定》;酸价的测定参照GB 5009.229-2016《食品安全国家标准 食品中酸价的测定》;碘值的测定参照GB/T 5532-2022《动植物油脂碘值的测定》;皂化值的测定参照GB/T 5534-2008《动植物油脂皂化值的测定》;水分的测定参照GB 5009.3-2016《食品安全国家标准 食品中水分的测定》;丙二醛采用ELISA试剂盒进行测定。
参考Ide[17]的方法并作适当修改。准确称取0.1 g油脂置于试管中,加入5 mL正己烷,振荡5 min使油脂完全溶解;随后加入2 mL 0.5 mol/L氢氧化钾甲醇溶液,充分摇匀后置于60 ℃水浴中加热30 min完成甲酯化反应。静置1 h后分层,取上清液通过0.22 µm有机滤膜以去除杂质。滤液用于气相色谱(Gas chromatography,GC)分析,进样量为1 µL。
参考Rebechi等[18]的分析条件并进行优化。Cd-2560毛细管气相色谱柱(100 m×0.25 mm×0.25 μm);载气为氮气;进样口温度为250 ℃,分流比为100:1,进样量为1 μL,升温程序为初始温度140 ℃,保持时间5 min;以4 ℃/min的升温速率升至240 ℃,保持时间30 min。通过37种脂肪酸甲酯混合标准品进行脂肪酸定性,脂肪酸相对百分比含量采用面积归一化法计算。每个样品平行测定3次,结果取平均值。
使用Excel 2024和SPSS 27.0软件对实验数据进行统计和单因素方差分析(one way ANOVA),使用Origin 2024进行作图,使用响应面Design-Expert 13软件进行响应面分析。各因素在相同条件下平行测定3次,实验统计数据以平均值±标准差表示。
经过观察可以发现,丙酮作为分提溶剂,油脂在20 ℃的养晶温度下开始结晶;异丙醇作为分提溶剂,油脂在30 ℃的养晶温度下开始结晶;正己烷和石油醚作为分提溶剂,油脂在15 ℃的养晶温度下开始结晶。分提所得固脂的得率及熔点变化如图1所示。正己烷和石油醚作为分提溶剂时结晶温度较低为15 ℃,所得固脂(正己烷15S、石油醚15S)得率显著低于丙酮组和异丙醇组(P<0.05),且晶体生长需要较长时间,因此这两种溶剂不适合作为分提溶剂使用。而丙酮组在20 ℃的养晶温度下结晶所得固脂(丙酮20S)得率为35.09%,固脂熔点为49.74 ℃,显著高于异丙醇组(P<0.05)。异丙醇组在30 ℃养晶温度下所得固脂(异丙醇30S)得率显著高于丙酮20S(P<0.05),但其熔点显著最低(P<0.05),为44.7 ℃。
为继续筛选异丙醇和丙酮两种溶剂并探究其对饱和脂肪酸的富集效果,养晶温度由30 ℃和20 ℃降低至25 ℃和15 ℃,养晶结束得到固脂(异丙醇25S和丙酮15S),检测这两种分提溶剂所得固脂的脂肪酸组成,结果如表3所示。可以发现在28S中添加溶剂后,丙酮20S的饱和脂肪酸由47.8%升高到63.21%,显著高于异丙醇组(P<0.05)。由图1可知,随着养晶温度的降低,丙酮组的固脂得率和熔点均无显著性变化,异丙醇组的固脂得率显著升高为56.21%(P<0.05)。通过对脂肪酸组成进行分析发现,降低养晶温度并没有显著提高丙酮组的饱和脂肪酸含量,但异丙醇25S的饱和脂肪酸含量显著降低(P<0.05)。因此,结合固脂得率、熔点及脂肪酸变化,选择丙酮作为分提溶剂进行后续实验。
从图2可以看出,油与溶剂比例对固脂得率和熔点有明显影响。固脂得率随着溶剂的增加呈现先上升后下降的变化,在1:1~1:4的油与溶剂比例下,固脂熔点显著升高(P<0.05)。在1:2的油与溶剂比例下,固脂得率显著最高(P<0.05),为33.79%,进一步增加溶剂添加量,固脂得率开始下降,当油与溶剂比例增加到1:4时,固脂熔点显著最高(P<0.05),当油与溶剂比例增加到1:5时,固脂得率和熔点均无显著变化,这一现象可能源于过多的丙酮导致溶液浓度变小,而结晶和晶体的生长需要合适的浓度差来推动,固脂的形成就会变慢,其中饱和脂肪酸的组成和含量也会达到相对稳定的状态,熔点也就相对稳定[19]。
酸价越低表明油脂的新鲜度越好,过氧化值越低表明油脂的氧化稳定性越好。从图2可以看出,油与溶剂比例对固脂过氧化值和酸价均有明显影响。过氧化值和酸价均呈现先下降后上升的变化,在油与溶剂比例为1:2时,过氧化值和酸价显著最低(P<0.05),分别是0.025 mg/g和0.6 mg/g,潜在原因是当油与溶剂为1:2时,丙酮对固脂中的氧化产物溶解度更高,造成了氢过氧化物的分解,且分解速度大于其生成速度,同时游离脂肪酸也被丙酮溶解,从而有效降低酸价和过氧化值[20]。比例过低,游离脂肪酸和氧化产物无法被充分溶解;比例过高,丙酮难以完全回收,残留溶剂可能催化后续的氧化反应,从而增加氧化酸败的风险。
综合上述结果,选择油与溶剂比例1:2作为最适比例开展后续实验。
从图3可以看出,养晶温度对固脂得率和熔点有明显影响。23 ℃养晶温度下的固脂得率和熔点显著低于20 ℃养晶温度下的固脂得率及熔点(P<0.05),且在20 ℃养晶温度下固脂得率和熔点均显著最高(P<0.05),得率从26.1%升高到34.09%,熔点从49.03 ℃升高到50.23 ℃。继续降低养晶温度,固脂的得率无显著变化,固脂熔点继续降低,其主要原因在于较低的养晶温度会造成体系黏度增加,脂肪酸在该环境中移动困难,减缓晶体的生长,导致固脂得率不再显著变化[21];较低的养晶温度也会导致部分熔点较低的甘油三酯进入固脂,使固脂的饱和脂肪酸含量降低,固脂熔点也随之下降[22]。在23~20 ℃的养晶温度范围内固脂的得率和熔点均显著增加(P<0.05),说明在该温度范围内分提工艺对高熔点固脂的影响最大,合适的养晶温度可以提高分提效率,一定程度上减少工业生产过程中形成的误差。
油脂中多不饱和脂肪酸含量越高,越易氧化[23]。观察图3可以发现,养晶温度对固脂过氧化值和酸价均有明显影响。23 ℃养晶温度下,过氧化值和酸价最高,养晶温度降低到20 ℃时,过氧化值和酸价显著降低(P<0.05),过氧化值从0.034 mg/g降低到0.025 mg/g,酸价从0.69 mg/g降低到0.59 mg/g。继续降低养晶温度,过氧化值和酸价均无显著变化。这可能是因为在20 ℃养晶温度下,高熔点饱和甘油三酯优先结晶,游离脂肪酸和多不饱和脂肪酸保留在液相中,导致固脂氧化稳定性较高,继续降温,导致部分中熔点、低熔点甘油三酯可能共结晶带入少量的多不饱和脂肪酸,但由于油与溶剂比例已经固定为1:2,影响有限,所以继续降温,其过氧化值和酸价无显著变化。在薛淼等[24]的研究中,鸡油加工储藏过程中,温度过高会导致油脂的品质下降,过氧化值降低、同时也会导致蛋白质变性程度增大,脂酶活性下降,分解脂肪能力减弱,酸价降低,造成油脂酸败变质。这与上述研究结果一致。
综合上述结果,选择养晶温度20 ℃作为最适养晶温度开展后续实验。
合适的降温速率可以保证油脂在分提过程中形成最稳定的晶型。如果采用温差过大的急骤冷却,易使油脂中形成无法分离的玻璃脂质体,快速冷却会促进不稳定多晶型物的结晶而形成晶束,导致结晶的互溶性和选择性差,只有通过缓慢冷却至一定的结晶温度,才能得到相应的晶型[25]。从图4可以看出,不同的降温速率对固脂的得率有显著影响,但对固脂熔点无显著影响。在4 ℃/h的降温速率下,固脂得率显著低于其他组(P<0.05),这是因为过慢的降温速率造成晶核生成和晶体生长的时间延长,固液相不易分离而降低了固脂得率;在6 ℃/h的降温速率下固脂得率最高,继续增加降温速率固脂得率逐渐减小,但并无显著变化,主要归因于8~12 ℃/h降温范围内,降温速率过快,导致晶体成核过冷,晶核瞬间形成,养晶时间不足以支撑晶体的充分成长,造成晶体分布不均匀,体系黏度增大,但丙酮的加入在一定程度上降低体系黏度,增强分子扩散,使高熔点甘油三酯仍能有序的结晶,减少了液相包裹,使固脂得率和熔点维持在稳定状态,不再显著变化。张东明等[26]在一次干法分提和二次干法分提制备液态猪油过程中所得研究结论与此基本相符。
过氧化值反映的是油脂初级氧化产物(过氧化物)的积累量。从图4可以发现,降温速率4 ℃/h时的过氧化值显著高于6 ℃/h时的过氧化值(P<0.05),因为以4 ℃/h降温速率降温时,温度下降缓慢,晶体生长时间充足,易形成粗大的固脂晶体。这类晶体结构疏松,会吸附更多液脂,同时由于体系长时间处于中低温过渡阶段,可能会导致过氧化物的生成[27];当降温速率为8 ℃/h时,过氧化值显著最低(P<0.05),为0.024 mg/g,这可能是因为在8 ℃/h的降温速率下,形成细小且紧密的固脂晶体结构,有效减少液脂残留,导致不饱和脂肪酸含量不足以支撑固脂发生氧化反应,且降温速率适中,避免其长时间处在中低温过渡阶段,减少了过氧化物的产生,显著降低了过氧化值(P<0.05);当降温速率在10~12 ℃/h的范围内,温度下降过快,晶体未进行有序排列而形成细小且不规则的晶体,与氧气、溶剂的接触面积变大,促进固脂晶体表面的不饱和脂肪酸氧化,从而导致过氧化值的增加,同时,在8 ℃/h降温速率下所得固脂的酸价也达到最低,为0.55 mg/g,继续增加降温速率,酸价无显著变化,猜测可能是因为极性溶剂丙酮对游离脂肪酸的溶解度远高于对非极性甘油三酯的溶解度,导致固脂中的游离脂肪酸极少,不会对酸价造成显著影响[28]。
综合上述结果,选择降温速率8 ℃/h作为最适降温速率开展后续实验。
油脂的结晶过程包括晶核的形成和晶体生长2个阶段,从晶核的形成到晶体的生长需要一定时间才会形成稳定的晶体形态[29]。从图5可以看出,随着养晶时间的增加,固脂得率呈现先显著上升后缓慢下降的变化,固脂熔点变化平缓。3~9 h养晶时间下的固脂得率显著上升(P<0.05),12 h的养晶时间下固脂得率最大,从32.04%升高到33.40%,继续增加养晶时间,固脂得率无显著变化,引起这种现象的原因是3~9 h的养晶时间过短,晶体生长还没有达到稳定状态,高熔点甘油三酯还没有结晶充分,导致3~9 h养晶时间下的固脂得率在不断上升,当养晶时间为12 h时,固脂得率显著最大(P<0.05),此时晶体生长已经达到稳定状态,继续增加养晶时间,固脂得率缓慢下降,但并无显著性差异。贾晓童[30]在对羊油干法分提过程中,固脂得率和熔点也有相似变化,表明养晶时间过长会导致部分不饱和脂肪酸形成结晶进入固脂晶体,造成固脂得率缓慢下降,同时养晶时间过长还可能会降低固脂的氧化稳定性[31]。
随着养晶时间的增加,固脂的过氧化值呈现先下降后上升的变化,在12 h的养晶时间下,其过氧化值最低,为0.02 mg/g,继续增加养晶时间其过氧化值显著升高(P<0.05)。养晶时间为3 h时,固脂晶体较小,晶体状态不稳定,易吸附不饱和脂肪酸,导致过氧化物的生成底物充足。随着养晶时间的增加,固脂晶体达到稳定状态,会优先保留饱和脂肪酸,而多不饱和脂肪酸则会更多的存在液相中,减少了固脂的氧化底物,同时,固脂晶体对脂溶性的抗氧化物质包裹能力增强,抑制过氧化物生成,从而导致过氧化值显著降低(P<0.05)。当养晶时间大于12 h时,养晶时间过长,可能会导致原本包裹的抗氧化物质释放到液相中,固脂抗氧化能力降低,导致过氧化值显著增加(P<0.05)[32]。养晶时间为12 h的酸价与过氧化值相似,达到最低,为0.44 mg/g,继续增加养晶时间,酸价无显著变化,说明12 h的养晶时间下油脂品质较好。
在后续的优化过程中,需要综合考虑养晶时间这一关键因素,合理地控制养晶时间可以提高固脂的纯度以及品质,从而实现最佳的分提固脂效果。
根据前期单因素实验结果,运用Design-Expert 13软件进行Box-Behnken响应面试验对分提工艺进一步优化,响应面试验设计与结果见表4,方差分析结果见表5。
对表4中的实验数据进行回归分析,利用Design-Expert 13对油与溶剂比例(A)、养晶温度(B)、降温速率(C)、养晶时间(D)与各评价指标的综合评分(Y)进行二项式拟合,得到拟合方程为:
Y=93.81−2.84A−2.11B−0.96C+0.50D−1.14AB−1.05AC+0.66AD+1.43BC−0.08BD+0.42CD−11.86A2−7.79B2−7.44C2−8.58D2
决定系数R2=0.9924、校正系数Radj2=0.9849说明最佳工艺条件下试验值与模型预测值拟合较好[33]。对模型进行方差分析,由表5可知,回归模型P<0.0001,同时失拟项不显著(P=0.8902>0.05),说明拟合方程的预测值与实际值有较好的相关性,不确定因素并未对模型的构建产生显著影响,因此该模型拟合良好[34],可以有效地反映因素对综合评分的影响。各因素对综合评分的影响顺序为:油与溶剂比例(A)>养晶温度(B)>降温速率(C)>养晶时间(D);观察各因素的P值可以发现一次项A、B、C均呈现极显著影响(P<0.01),二次项A2、B2、C2、D2具有极显著影响(P<0.01),模型中的交互项AB、AC影响显著(P<0.05),BC影响极显著(P<0.01),表明因素与综合评分之间并非只是单一的线性关系。
干法分提协同溶剂法工艺优化的3D响应面图和等高线图可以直观地反映油与溶剂比例、养晶温度、降温速率、养晶时间对综合评分的影响及交互作用。曲面越陡,等高线越密集,影响越显著;等高线呈圆形表明两因素之间交互作用不明显,等高线呈明显椭圆表明两因素之间交互作用明显[35−36]。本模型的3D响应面图和等高线图见图6。由图可知,AB、AC、BC的响应面图曲面比较陡,等高线密集呈现椭圆,说明油与溶剂比例与养晶温度、油与溶剂比例与降温速率、养晶温度与降温速率交互作用较强,对综合评分影响显著;AD、BD、CD响应面图平缓,等高线稀疏且呈现圆形,表明油与溶剂比例与养晶时间、养晶温度与养晶时间、降温速率与养晶时间交互作用不明显,对综合评分的影响较弱。上述分析结果与方差分析中各交互项的显著性检验结果一致。
通过Design-Expert 13预测处理得到最佳结果,预测所得最佳分提工艺条件为:溶剂与油比例1:1.891,养晶温度19.599 ℃,降温速率7.863 ℃/h,养晶时间12.075 h,综合评分为94.146。考虑到实际操作的可行性,将最佳分提工艺参数调整为:溶剂与油比例1:2,养晶温度20 ℃,降温速率8 ℃/h,养晶时间12 h。在该条件下,进行3次验证实验,分提所得固脂得率为33.23%、熔点为50.1 ℃、过氧化值为0.02 mg/g、酸价为0.42 mg/g、综合评分为93.88,结果见表6,相对标准偏差(RSD)为0.42%,表明实际值与预测值非常接近,说明该工艺条件稳定,重复性好,具有实际应用价值。
对分提前后羊臀脂的理化性质进行分析检测,结果见表7,可知分提后得到的28S和20S的各项理化指标相较于原脂均有显著变化(P<0.05)。28S与原脂相比,过氧化值显著降低为0.048 mg/g(P<0.05);酸价显著降低为0.54 mg/g(P<0.05);丙二醛显著降低为2.18 nmol/mL(P<0.05),与过氧化值和酸价的变化结果一致;碘值显著降低为46.72 g/100 g(P<0.05);皂化值降低为197.65 mg/g(P<0.05)。干法分提协同溶剂法得到的20S与28S相比,过氧化值从0.048 mg/g显著降低为0.025 mg/g(P<0.05);酸价从0.54 mg/g显著降低为0.44 mg/g(P<0.05),远低于GB 10146-2015《食品安全国家标准 食用动物油脂》最高限(2.50 mg/g和2 mg/g)[37];丙二醛从2.18 nmol/mL显著降低为1.94 nmol/mL(P<0.05),说明相较于干法分提,溶剂的加入显著提高了高熔点羊油组分的氧化稳定性,碘值从46.72 g/100 g显著降低为42.42 g/100 g(P<0.05),表明溶剂的加入更利于固脂的结晶,显著提高了高熔点羊油组分的饱和程度,这与表8饱和脂肪酸的变化趋势一致;皂化值从197.65 mg/g显著降低为195.38 mg/g(P<0.05),碘值的降低会提高20S的饱和脂肪酸含量,从而使其平均相对分子量更高,导致皂化值相对较低,皂化性较好[38]。综合以上分析可知,阿勒泰羊臀脂经干法分提协同溶剂法分提得到的高熔点羊油组分的各项理化指标均有显著变化,油脂品质较好。
分提前后羊臀脂中的主要脂肪酸组成及含量如表8所示,可以发现一共检测出12种脂肪酸。原脂中棕榈酸、硬脂酸等饱和脂肪酸占比约43.94%;油酸、棕榈油酸等不饱和脂肪酸占比约53.25%。分提得到的28S和20S与原脂相比饱和脂肪酸含量都显著升高(P<0.05),分别升高了3.86%、19.27%,说明该分提工艺可以显著富集固脂中的饱和脂肪酸。28S与原脂相比,主要饱和脂肪酸的含量均有显著变化:肉豆蔻酸升高了0.14%,棕榈酸升高了1.26%,硬脂酸升高了2.28%;主要不饱和脂肪酸也有相似的显著变化(P<0.05):油酸降低了2.99%,亚油酸降低了0.32%,这是因为饱和脂肪酸熔点较高,在冷却过程中先析出晶体形成固脂,从而使得到的固脂中的饱和脂肪酸含量增加,说明干法分提在提升固脂饱和度方面有一定作用,研究人员[39−40]均在干法分提过程中得到一致研究结果。20S与28S相比,饱和脂肪酸含量进一步升高,从47.8%升高到63.21%,呈显著差异(P<0.05),其中肉豆蔻酸从2.87%升高到3.13%,棕榈酸由23.36%升高到27.86%,硬脂酸从16.95%升高到27.01%;不饱和脂肪酸显著降低(P<0.05),从49.61%降低到34.61%,其中油酸从36.56%降低到25.37%,棕榈油酸从2.79%降低到2.19%,亚麻酸从1.38%降低到0.91%。分提前后主要变化的脂肪酸是硬脂酸、棕榈酸和油酸,这是因为硬脂酸和棕榈酸熔点较高,油酸熔点较低,因此在分提后固脂中的含量呈显著变化,符合其他研究者的观点[41]。相较于单一的干法分提所得高熔点羊油组分,干法分提协同溶剂法使饱和脂肪酸被进一步高度富集,溶剂的加入提高了分提效率,得到更高纯度的高熔点羊油组分,Zhang等[42]研究发现高熔点分提组分具有很好的延展性,适合开发高温煎炸油、起酥油、代可可脂等特种油脂和更高附加值的产品。因此,高熔点羊油组分具有独特的应用价值。
本研究通过单因素与响应面试验,以固脂得率、熔点、过氧化值和酸价为指标优化干法分提协同溶剂法分提工艺,并对比分析分提前后羊臀脂的理化特性与脂肪酸组成变化。结果表明:分提工艺最佳条件为油与溶剂比例1:2、养晶温度20 ℃、降温速率8 ℃/h、养晶时间12 h,在此条件下分提所得固脂得率为33.23%、熔点为50.1 ℃、过氧化值为0.02 mg/g、酸价为0.42 mg/g、综合评分为93.88。分提所得高熔点羊油组分各项理化指标表现较好,氧化稳定性有明显提升,符合食用动物油的食品安全国家标准;相较于单一干法分提,干法分提协同溶剂法分提工艺可以更为显著地富集饱和脂肪酸,所得高熔点羊油组分的饱和脂肪酸含量升高到63.21%,显著提高15.41%(P<0.05),为富集饱和脂肪酸提供新思路,同时为高附加值的羊油副产品及特殊用途油脂的深入开发与合理应用提供理论依据。

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2026年第47卷第13期
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doi: 10.13386/j.issn1002-0306.2025080245
  • 接收时间:2025-08-25
  • 首发时间:2026-10-24
  • 出版时间:2026-07-01
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  • 收稿日期:2025-08-25
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    新疆农业大学食品科学与药学学院,新疆乌鲁木齐 830052

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王子荣(1963−),男,博士,教授,研究方向:食品营养与安全,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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