GC-MS分析食用油中甘油三酯的研究进展

介绍了GC-MS分析食用油中甘油三酯的几种情况,包括高温气相色谱(300℃)直接进样,将甘油三酯进行甲酯化处理的非高温气相色谱(300℃)非直接进样。并介绍了GC-氢离子火焰检测器直接进样和非直接进样技术。指出了这些技术在食用油甘油三酯的分析上取得的进展和存在的一些问题。     

Lipase‐catalyzed production of biodiesel from rice bran oil

Biodiesel has attracted considerable attention as an alternative fuel during the past decades. The main hurdle to the commercialization of biodiesel is the cost of the raw material. Use of an inexpensive raw material such as rice bran oil is an attractive option to lower the cost of biodiesel. Two commercially available immobilized lipases, Novozym 435 and IM 60, were employed as catalyst for the reaction of rice bran oil and methanol. Novozym 435 was found to be more effective in catalyzing the methanolysis of rice bran oil. Methanolysis of refined rice bran oil and fatty acids (derived from rice bran oil) catalyzed by Novozym 435 (5% based on oil weight) can reach a conversion of over 98% in 6 h and 1 h, respectively. Methanolysis of rice bran oil with a free fatty acid content higher than 18% resulted in lower conversions (<68%). A two‐step lipase‐catalyzed methanolysis of rice bran oil was developed for the efficient conversion of both free fatty acid and acylglycerides into fatty acid methyl ester. More than 98% conversion can be obtained in 4–6 h depending on the relative proportion of free fatty acid and acylglycerides in the rice bran oil. Inactivation of lipase by phospholipids and other minor components was observed during the methanolysis of crude rice bran oil. Simultaneous dewaxing/degumming proved to be efficient in removing phospholipids and other minor components that inhibit lipase activity from crude rice bran oil. Copyright © 2005 Society of Chemical Industry     

Single-Walled Carbon Nanohorns as Boosting Surface for the Analysis of Low-Molecular-Weight Compounds by SALDI-MS

Limits of Matrix-Assisted Laser Desorption Ionization (MALDI) mass spectrometry (MS) in the study of small molecules are due to matrix-related interfering species in the low m/z range. Single-walled carbon nanohorns (SWCNH) were here evaluated as a specific surface for the rapid analysis of amino acids and lipids by Surface-Assisted Laser Desorption Ionization (SALDI). The method was optimized for detecting twenty amino acids, mainly present as cationized species, with the [M+K]⁺ response generally 2-time larger than the [M+Na]⁺ one. The [M+Na]⁺/[M+K]⁺ signals ratio was tentatively correlated with the molecular weight, dipole moment and binding affinity, to describe the amino acids’ coordination ability. The SWCNH-based surface was also tested for analyzing triglycerides in olive oil samples, showing promising results in determining the percentage composition of fatty acids without any sample treatment. Results indicated that SWCNH is a promising substrate for the SALDI-MS analysis of low molecular weight compounds with different polarities, enlarging the analytical platforms for MALDI applications.     

Enzymatic interesterification of palm stearin with Cinnamomum camphora seed oil to produce zero-trans medium-chain triacylglycerols-enriched plastic fat

It is known that Cinnamomum camphora seed oil (CCSO) is rich in medium-chain fatty acids (MCFAs) or medium-chain triacylglycerols (MCTs). The purpose of the present study was to produce zero-trans MCTs-enriched plastic fat from a lipid mixture (500 g) of palm stearin (PS) and CCSO at 3 weight ratios (PS:CCSO 60:40, 70:30, 80:20, wt/wt) by using lipase (Lipozyme TL IM, 10% of total substrate) as a catalyst at 65 °C for 8 h. The major fatty acids of the products were palmitic acid (C16:0, 42.68% to 53.42%), oleic acid (C18:1, 22.41% to 23.46%), and MCFAs (8.67% to 18.73%). Alpha-tocopherol (0.48 to 2.51 mg/100 g), γ-tocopherol (1.70 to 3.88 mg/100 g), and δ-tocopherol (2.08 to 3.95 mg/100 g) were detected in the interesterified products. The physical properties including solid fat content (SFC), slip melting point (SMP), and crystal polymorphism of the products were evaluated for possible application in shortening or margarine. Results showed that the SFCs of interesterified products at 25 °C were 9% (60:40, PS:CCSO), 18.50% (70:30, PS:CCSO), and 29.2% (80:20, PS:CCSO), respectively. The β' crystal form was found in most of the interesterified products. Furthermore, no trans fatty acids were detected in the products. Such zero-trans MCT-enriched fats may have a potential functionality for shortenings and margarines which may become a new type of nutritional plastic fat for daily diet.     

中链甘油三酯微胶囊的体外释放及对小鼠脂质代谢的影响

采用喷雾干燥技术制备中链甘油三酯微胶囊,将中链甘油三酯固态化,方便食品添加和储运;以人工胃液模拟体外释放,初步研究了中链甘油三酯微胶囊的缓释特性;并以基础合成饲料、长链甘油三酯微胶囊高脂饲料(长链甘油三酯供能占总能量30%左右)和中链甘油三酯微胶囊高脂饲料(中链甘油三酯供能占总能量30%左右)分别饲喂小鼠,并观察5周内小鼠健康状况和体质量、血清甘油三酯(TG)、总胆固醇(TC)、高密度脂蛋白胆固醇(HDL-C)含量、低密度脂蛋白胆固醇(LDL-C)含量、饲料消耗量的变化,研究中链甘油三酯对小鼠脂质代谢的影响。结果表明,中链甘油三酯微胶囊在人工胃液中可缓慢释放6h,能够缓解中链甘油三酯一次性摄入量超标引起的腹痛腹泻问题,膳食中添加中链甘油三酯微胶囊后,能降低体内TC和LDL-C的含量,中链甘油三酯微胶囊的高脂膳食具有预防肥胖、减少体质量增长和体脂累积、减轻肝脏脂肪沉积的作用,且其抑制体质量增长的机制与减少能量摄入量无关。     

胰脂肪酶催化樟树籽仁油和甘油合成中碳链单甘油酯

采用胰脂肪酶催化樟树籽仁油与甘油反应合成中碳链单甘油酯,通过单因素试验和正交试验,研究了反应时间、加酶量、醇油摩尔比、反应初始加水量、反应温度对产物中中碳链单甘油酯含量的影响。结果表明,胰脂肪酶催化樟树籽仁油(10 mL)与甘油反应合成中碳链单甘油酯的适宜条件为:反应温度47℃,加酶量220 mg,醇油摩尔比4.3∶1,反应初始加水量35μL,反应时间30 h。在此反应条件下,产物中中碳链单甘油酯的含量为53.42%±0.05%。     

中链甘油三酯微胶囊的理化性质表征

从理化性质和感官指标上对实验制得的中链甘油三酯微胶囊产品进行评价。结果显示:制得的中链甘油三酯微胶囊产品,其气味纯正、无异味;颜色洁白;平均粒径为244.20 nm;颗粒均匀、呈圆球状,对芯材保护效果较好;水分含量为2.65%,溶解度为97.60%。差示扫描量热分析结果表明,中链甘油三酯微胶囊在温度低于90℃的加工中能够稳定存在。红外光谱分析证实,中链甘油三酯受微胶囊化的影响不大,能基本保留原有结构。     

Br?nsted酸性离子液体催化合成辛酸甘油酯的研究

以双磺基的Brnsted酸性离子液体1-磺酸丁基-3-甲基咪唑硫酸氢盐[MIm(CH2)4SO3H][HSO4)]催化辛酸与甘油酯化合成低热量的中碳链三酰甘油,研究了催化剂用量、酸醇物质的量比、反应温度、反应时间对酯化反应的影响,在最优条件下考查了工艺稳定性及催化剂重复使用性能。结果表明,[MIm(CH2)4SO3H][HSO4]具有较高的酯化催化活性和重复使用性能。优化的合成辛酸甘油酯的工艺条件为:辛酸甘油物质的量比为3.5∶1,催化剂用量为底物质量的1%,反应温度160℃,反应时间6 h。在此条件下,酯化率达85%,三酰甘油质量分数达到80%。催化剂重复使用5次,仍保持90%的催化活性。     

高效体积排阻色谱测定油脂中氧化甘油三酯聚合物

为了分析甘油三酯氧化产物——氧化甘油三酯及其聚合物的组分分布,研究了高效体积排阻色谱检测高相对分子质量聚合物的方法,建立了采用正相硅胶制备色谱预分离油脂中极性组分,极性组分以高效体积排阻色谱-示差折光检测器测定,标准相对分子质量聚苯乙烯定性,峰面积归一化法定量的检测方法.油脂中极性组分的典型色谱峰构成是:氧化甘油三酯寡聚合体、氧化甘油三酯二聚体、氧化甘油三酯单体、甘油二酯、游离脂肪酸等.以氧化甘油三酯聚合物鉴别地沟油等深度氧化劣变食用油具有良好的应用前景.     

中链脂肪酸-VC复合脂质体制备及初步稳定性

以磷脂和胆固醇为膜材,脂溶性的中链脂肪酸(MCFAs)和水溶性的VC为模型药物,以脂质体的包封率和粒径为指标,分别采用薄膜法、复乳法、薄膜-高压法、复乳-高压法制备中链脂肪酸-VC复合脂质体,筛选出最佳制备方法(复乳-高压法),并通过单因素试验设计,确定复合脂质体的最优处方工艺为:总脂材质量浓度5.0g/100mL,MCFAs质量浓度10.0mg/mL,VC质量浓度3.0mg/mL,卵磷脂与胆固醇质量比为4:1,卵磷脂质量与无水乙醇体积比为1:10(g/mL),吐温与总脂材质量比为3:10,VE与卵磷脂质量比为4:100,120MPa条件下超微乳化处理2次。制备的复合脂质体MCFAs包封率达到49.01%,VC的包封率达到54.19%,平均粒径90.3nm,在4℃贮藏15d,包封率和粒径变化不大,表明脂质体低温贮藏稳定性良好。