石榴籽油中的石榴酸分析方法研究

以石榴籽油为研究对象,通过气相色谱-质谱联用(GC-MS)对其脂肪酸含量及组成进行了分析,研究了不同甲酯化方法对石榴酸和其他脂肪酸含量的影响。试验表明,石榴籽油中含丰富石榴酸(74%)。经薄层色谱(TLC)验证,酸、碱催化法都可使石榴籽油完全甲酯化,但酸催化(三氟化硼-甲醇)会导致石榴酸的共轭双键构型发生顺反异构,使石榴酸向其共轭化合物转化,降低了其在终产物中的含量。结果表明,对于像石榴籽油一样富含共轭脂肪酸的油类物质,应选用碱催化法进行甲酯化。     

气—质联用测定新疆石榴籽油中脂肪酸含量

对石榴籽油中的脂肪酸成分进行测定研究。通过氢氧化钾-甲酯酯化反应,以十一烷酸甲酯为内标物,正己烷为萃取溶剂,采用气相色谱—质谱联用技术对石榴籽油中脂肪酸甲酯成分进行分析,辅助NIST库检索并分析各组分。建立内标法测定石榴籽油中脂肪酸含量的方法。结果表明,石榴籽油中主要成分为石榴酸,其含量超过70%(w/w)。该方法前处理简便快捷,结果准确度高,分析时间较短,可为内标法测定脂肪酸含量提供借鉴。     

石榴籽油低温连续相变萃取工艺优化及其脂肪酸分析

采用低温连续相变萃取技术分离石榴籽油,以油脂得率为指标,通过正交试验L9(3~4)优化萃取工艺,并对石榴籽油理化性质和脂肪酸组成进行分析。结果表明,低温连续相变萃取石榴籽油的最佳工艺条件为:原料颗粒度60目,萃取压力0.5 MPa,萃取温度45℃,萃取时间70 min,解析温度70℃,该条件下石榴籽油得率为15.94%,石榴籽原料含油量16.31%,提取回收率高达97.60%。低温连续相变萃取石榴籽油呈浅黄色半固体膏状物,酸价为3.26 mg KOH/g,过氧化值为0.10g/100g。石榴籽油主要脂肪酸组成为9C,11TR,13TR-十八碳三烯酸甲酯(亚油酸,68.09%)、亚油酸甲酯(9.13%)、十八烯酸甲酯(6.91%)、棕榈酸甲酯(4.73%)、硬脂酸甲酯(3.33%)。     

超临界CO2萃取石榴籽油及石榴酸甲酯富集

采用超临界CO2 萃取技术从石榴籽中提取石榴籽油,对其脂肪酸和甘三酯组成和含量进行分析;通过单因素和正交优化试验研究尿素包合法富集石榴酸甲酯。超临界CO2 萃取技术与有机溶剂萃取相比更有利于获得高石榴酸含量的石榴籽油,石榴籽油中检测出14 种甘三酯。尿素包合法富集石榴酸甲酯的最佳工艺为尿素包合温度5 ℃、包合时间20 h、尿素与脂肪酸甲酯的质量比1∶1、尿素和95%乙醇的质量比1∶5,此最佳包合条件下获得的石榴酸甲酯的含量为78.82%。     

分子蒸馏富集石榴籽油脂肪酸乙酯中共轭亚麻酸乙酯的研究

采用分子蒸馏技术对石榴籽油脂肪酸乙酯中的共轭亚麻酸乙酯进行富集。通过单因素实验,对影响分子蒸馏纯化共轭亚麻酸乙酯的4个因素,即预热温度、进料速率、刮板转速和蒸馏温度进行了优化,然后经过两级分子蒸馏富集共轭亚麻酸乙酯。在工作压力为1.0×10-3k Pa的条件下,最终确定了纯化共轭亚麻酸乙酯的最佳工艺条件为:预热温度70℃,进料速率2 m L/min,刮板转速120 r/min,一级蒸馏温度120℃和二级蒸馏温度160℃。在最佳工艺条件下,共轭亚麻酸乙酯含量从蒸馏前的80.68%提升到了95.23%。     

不同甲酯化方法对瓜蒌籽油中十八碳三烯酸种类和含量的影响

以索氏抽提的瓜蒌籽油为原料,测定其酸值、碘值和皂化值。分别采用酸催化法、碱催化法和BF3催化法对瓜蒌籽油进行甲酯化处理,利用气相色谱-质谱联用仪分析其脂肪酸中十八碳三烯酸的种类和含量。结果表明：瓜蒌籽油酸值为0.51 mg KOH/g,碘值为1.3398 g I2/g,皂化值为1.9143 g KOH/g。酸催化法鉴定出5种十八碳三烯酸,为栝楼特征性脂肪酸-瓜蒌酸、梓树酸、α-桐酸、γ-亚麻酸和α-亚麻酸,含量分别为6.43%、9.5%、7.00%、5.82%和1.52%;碱催化法和BF3催化法均鉴定出4种,为瓜蒌酸、α-桐酸、梓树酸和α-亚麻酸,其含量分别为31.24%和27.17%、3.33%和3.56%、1.23%和2.02%和0.38%和0.78%。结论：瓜蒌籽油品质符合国家食用油标准,可进一步开发利用;碱催化甲酯化法对十八碳三烯酸的异构效应最小,更适合用于瓜蒌籽油脂肪酸分析。     

牡丹种皮、种子及4种干果油脂的脂肪酸组成分析

目的明确牡丹种皮油的脂肪酸组成及相对含量,并与牡丹籽油和4种常见干果(核桃、巴旦木、杏仁、开心果)的脂肪酸组成进行比较,为牡丹种皮油的开发利用提供科学依据。方法采用索氏抽提法对4种干果中的脂肪进行提取,以硫酸-甲醇法对6种油脂样品甲酯化,采用GC-MS检测结合峰面积归一化法测定脂肪酸的组成及相对含量。结果牡丹种皮油与牡丹籽油中均含有棕榈酸、棕榈油酸、油酸、亚油酸、亚麻酸5种脂肪酸,其不饱和脂肪酸比例均超过90%,尤其是亚麻酸的含量分别高达51.1%和44.7%;而核桃中含有棕榈酸、油酸、亚油酸、亚麻酸4种脂肪酸,亚油酸是其主要成分;巴旦木、杏仁、开心果中主要含有棕榈酸、油酸、亚油酸3种脂肪酸,以单不饱和脂肪酸油酸含量最高。结论牡丹种皮油中含有大量多不饱和脂肪酸,其中亚麻酸的含量尤其突出,较牡丹籽油含量更高,是一种优质的保健食用油。     

响应面法优化超临界CO_2萃取栝楼籽油

通过响应面法(response surface methodology)优化超临界二氧化碳萃取栝楼籽油工艺,采用DesignExpert软件对试验数据进行分析,气相色谱-质谱(gas chromatography-mass spectrometry)对萃取栝楼籽油进行成分分析。结果表明,最佳工艺参数为萃取压力29.75 MPa,萃取温度45.1℃,萃取时间为175.8min,栝楼籽油萃取得率为32.82%,栝楼籽油主要成分为棕榈酸(7.90%)、α-亚麻酸(28.23%)、亚油酸(39.33%)和油酸(22.57%)为主,另外检出不饱和脂肪酸7-棕榈烯酸(0.40%)、γ-亚麻酸(0.22%)和11-二十碳烯酸(0.30%),同时检出不饱和烃类角鲨烯(0.33%)。萃取时间、萃取压力、萃取温度对栝楼籽油超临界CO_2萃取工艺有显著的影响,栝楼籽油不饱和脂肪酸质量分数达90.59%。     

牡丹种皮、种子及几种干果油脂的脂肪酸组成分析

摘 要: 目的 明确牡丹种皮油的脂肪酸组成及相对含量,并与牡丹籽油和4种常见干果（核桃、巴旦木、杏仁、开心果）的脂肪酸组成进行比较,为牡丹种皮油的开发利用提供科学依据。方法 采用索氏抽提法对4种干果中的脂肪进行提取,以硫酸-甲醇法对6种油脂样品甲酯化,采用GC-MS检测结合峰面积归一化法测定脂肪酸的组成及相对含量。 结果 牡丹种皮油与牡丹籽油中均含有棕榈酸、棕榈油酸、油酸、亚油酸、亚麻酸5种脂肪酸,其不饱和脂肪酸比例均超过90%,尤其是亚麻酸的含量分别高达51.1%和44.7%;而核桃中含有棕榈酸、油酸、亚油酸、亚麻酸4种脂肪酸,亚油酸是其主要成分;而巴旦木、杏仁、开心果中主要含有棕榈酸、油酸、亚油酸3种脂肪酸,以单不饱和脂肪酸油酸含量最高。 结论牡丹种皮油中含有大量多不饱和脂肪酸,其中亚麻酸的含量尤其突出,较牡丹籽油含量更高,是一种优质的保健食用油。     

杜仲籽油中α-亚麻酸的甲酯化方法优化

以超临界CO2萃取的杜仲籽油为原料,对其主要成分α-亚麻酸的甲酯化方法进行筛选和优化.在确定合适的α-亚麻酸甲酯化方法基础上,考察了催化剂用量、催化剂浓度、反应温度、反应时间等对α-亚麻酸甲酯化效果的影响,确定最佳的甲酯化条件为:用2 mL石油醚－苯(V(石油醚):V(苯)=1:1)为溶剂将0.2 g 杜仲籽油溶解,加入5 mL 0.2 mol/L的KOH－甲醇溶液作催化剂,反应温度50℃,反应时间30 min.薄层展开检识显示在该条件下,杜仲籽油中α-亚麻酸甲酯化反应完全,气相色谱检测表明甲酯化率可达92.59%.     

栝楼籽油理化性质及其脂肪酸组成分析

用索氏提取法从栝楼籽中提取栝楼籽油,采用仪器分析和化学分析相结合的方法分析了栝楼籽油的理化特性、主要脂肪酸组成及甘三酯组成。结果表明,栝楼籽全籽含油量高达29.91%,不饱和脂肪酸含量达66.955%,其中栝楼酸含量高达16.15%。     

河南鹤壁瓜蒌子和瓜蒌皮中挥发油成分分析

采用减压蒸馏的方法提取瓜蒌子和瓜蒌皮中挥发油成分。采用气相色谱-质谱联用法对河南鹤壁瓜蒌子和瓜蒌皮中挥发油的化学成分进行分离和鉴定。从瓜蒌子共鉴定出13种化合物,主要为醛类(66.58%)、脂肪酸类化合物(12.4665%),还含有少量烃类(2.1819%)、醇类(3.922%)、酮类(2.4887%)、苷类(3.1607%)和三萜类化合物(2.1459%)等,其总和占挥发油的92.82%;从瓜蒌皮中鉴定得到26个化合物,主要为醛类(57.09%)、脂肪酸类(15.04%)、烃类(9.78%)、酮类(4.7%)等化合物,其含量之和占挥发油的93.03%。瓜蒌子和瓜蒌皮挥发油中均含(E,E)-2,4-壬二烯醛、2,4-癸二烯醛、(E)-2-庚烯醛、亚油酸、棕榈酸,角鲨烯。研究结果为瓜蒌类药材产品及食品添加剂的开发提供参考。     

瓜蒌籽油成分、提取方法及功能特性的研究进展

瓜蒌籽含油量高,油中以不饱和脂肪酸为主,其中特征性脂肪酸——栝楼酸和油脂中的微量成分具有多种生理功能。主要综述了瓜蒌籽油组成成分、提取方法及功能特性,对存在问题进行分析,并对前景进行展望,旨在为其进一步深入研究和开发利用提供理论参考。     

栝楼籽油清除自由基作用研究

以栝楼籽油清除羟基自由基能力和对超氧阴离子自由基的清除能力为指标,研究了栝楼籽油的抗氧化活性。实验表明栝楼籽油具有较好的清除超氧阴离子自由基的作用,最大抑制率为68.19%。栝楼籽油具有较好的清除羟自由基的作用,EC50为0.23mg/ml,具有明显的抗氧化作用。     

瓜蒌籽油理化性质及瓜蒌酸结构分析

对瓜蒌籽油的理化性质进行了测定,通过红外、紫外光谱法分析了瓜蒌籽油所含的特殊脂肪酸--瓜蒌酸的结构,并采用杂环化法衍生化瓜蒌籽油,应用气相色谱-质谱联用法对瓜蒌酸进行结构鉴定及含量测定,确定了瓜蒌酸的结构为C18:39c,11t,13c,采用峰面积归一化法计算出其质量分数为16.15%。     

Production of structured lipids containing conjugated linolenic acid: optimisation by response surface methodology

Structured lipids containing conjugated linolenic acid (CLNA) were produced separately by enzymatic acidolysis reaction of corn and canola oils (CAO) with bitter gourd (Momordica charantia L) seed oil fatty acids [bitter gourd seed oil fatty acids (BGFA)]. Reactions were conducted using a commercial immobilised sn‐1,3‐specific lipase from Thermomyces lanuginosa (Lipozyme TL IM) in hexane. The effects of reaction time, substrate molar ratio, temperature and enzyme amount on incorporation yield of CLNA were investigated and optimised by response surface methodology with three‐level, two‐factor face‐centred cube design. When reactions were conducted using 10% enzyme for 3 h, the optimum reaction conditions were found for corn oil (CO) as 53.5 °C and 5.9:1 BGFA/CO molar ratio. At these conditions, the incorporation of CLNA into CO was determined as 41.4%. However, CLNA incorporation into CAO was resulted as 37% at optimum conditions which were 54.2 °C and 6.8:1 BGFA/CAO molar ratio.     

贮藏温度对栝楼籽油脂酸败的影响

通过依据国家相关标准测定不同贮藏温度下栝楼籽的酸价、脂肪酶活动度、过氧化值、TBA 值及VE 的保留率以研究贮藏温度对栝楼籽油脂酸败的影响。结果表明：温度是影响栝楼籽油脂酸败的重要因素。在0℃和5℃的低温条件下,能明显抑制栝楼籽的脂肪酶活动度,降低酸价,延缓过氧化值和TBA 值的升高,减少VE 的消耗,有效延缓栝楼籽的油脂酸败。     

Physicochemical Properties and Volatile Profiles of Cold-Pressed Trichosanthes kirilowii Maxim Seed Oils

The physicochemical properties and volatile profiles of cold-pressed Trichosanthes kirilowii Maxim (T. kirilowii) seed oils from four regions in China were determined in this study. The total oil content and cold-pressed oil yield of the four different sourced seeds were 38.06–44.33% and 15.17–30.97%, respectively. All the cold-pressed oil samples were found to be rich in polyunsaturated fatty acids, with content ranging from 45.41 to 75.32% of the total fatty acids. Punicic, α-eleostearic and catalpic acids were the main conjugated linolenic acid isomers in the cold-pressed T. kirilowii seed oils. The results of melting and crystallization profiles indicated that each oil sample exhibited different transitions steps due to its triacylglycerol composition, crystal structure and total unsaturation. Analysis of volatile profiles showed that 2,4-nonadienal was one of the most important aldehydes in the cold-pressed T. kirilowii seed oils, and less short chain acids (0.20%) but more esters (5.48%) were found in the sample with high content of punicic acid (Hebei sample). Results of oil quality indices indicated that cold-pressed T. kirilowii seed oils were liable to be oxidized, and their stabilities reduced with the increase of acid values. In general, more attention should be paid to improve the oxidative stability of cold-pressed T. kirilowii seed oils in their further application in food industry.     

刺梨籽油中脂肪酸成分的GC-MS分析

用超临界CO2流体提取刺梨籽油,经甲酯化处理,用气相色谱-质谱(GC/MS)联用技术对其脂肪酸的组成进行了分析和鉴定,并用面积归一化法测定了各种成分的质量分数。共分离鉴定了10种脂肪酸:含有4种饱和脂肪酸,占脂肪酸总量的14.91%,其中以棕榈酸(8.54%)、硬脂酸(4.42%)为主;含有6种不饱和脂肪酸,占总脂肪酸总量的83.64%,其中亚油酸(41.68%)、亚麻酸(25.44%)、油酸(12.74%)为主。刺梨籽油可作为一种富含不饱和脂肪酸的功能性油脂,该分析结果可为刺梨籽油的开发利用提供理论依据。     

Analysis of pomegranate seed oil for the presence of jacaric acid

BACKGROUND: Pomegranate seed oil is predominantly composed of triglycerides containing unsaturated fatty acids, including high levels of conjugated linolenic acids (CLnAs). The major CLnA component, punicic acid, is known to possess biological activity. Consequently, it is desirable to obtain a detailed characterisation of pomegranate seed oil fatty acid profiles, including molecules potentially co‐eluting with punicic acid, such as jacaric acid. RESULTS: Conjugated fatty acid profiles of a commercial sample of cold pressed pomegranate seed oil were characterised in detail by both gas chromatography of methyl esters and by ¹³C NMR spectroscopy. The methylation procedures were found to be critical for determination of accurate fatty acid profiles. GC analysis was unable to resolve jacaric acid from punicic acid, the major fatty acid present in pomegranate seed oil. To establish the presence or absence of jacaric acid, ¹³C NMR was employed. CONCLUSION: This is the first study to investigate pomegranate seed oil for the presence of jacaric acid. Punicic acid, eleostearic acid, and catalpic acid were confirmed by ¹³C NMR, but jacaric acid was not found. Thus, we have shown that punicic acid levels may be accurately measured by gas chromatography alone in pomegranate seed oil. Copyright © 2009 Society of Chemical Industry