超声波辅助稀碱水解法提取金鲳鱼骨油的工艺优化与脂肪酸组成分析

以金鲳鱼骨为原料,在对金鲳鱼骨中主要营养成分(水分、粗蛋白、粗脂肪和粗灰分)进行分析检测的基础上,利用单因素与正交试验相结合的方法优化金鲳鱼骨油稀碱水解(超声波辅助)法的提取工艺,并采用气相色谱-质谱法对最佳提取工艺所得的金鲳鱼骨油的脂肪酸组成进行测定分析,评价其营养价值。结果表明,金鲳鱼骨中水分、粗脂肪、粗蛋白和粗灰分质量分数分别为50.20%、29.97%、12.00%和7.63%。影响金鲳鱼骨油提取率的4个主要因素为液料比、p H值、提取温度和提取时间。当液料比为4∶1(m L/g)、p H 9、提取温度60℃、提取时间30 min、超声功率500 W时,金鲳鱼骨油的提取率为80.51%,该条件为稀碱水解(超声波辅助)法提取金鲳鱼骨油的最佳工艺参数。采用气相色谱-质谱联用技术对金鲳鱼骨油的脂肪酸进行定性、定量分析可知:金鲳鱼骨油中不饱和脂肪酸含量(68.44%)显著高于饱和脂肪酸含量(31.56%);单不饱和脂肪酸总量(37.99%)高于多不饱和脂肪酸总量(30.45%);其中油酸(27.86%)和棕榈酸(21.46%)含量最高,富含亚油酸、二十二碳六烯酸和二十碳五烯酸。金鲳鱼骨作为鱼类下脚料营养丰富,具有良好保健作用和经济价值,颇具开发利用前景。     

ω3-Fatty Acids in Some Fish Species from Turkey

ABSTRACT: The polyunsaturated ω3-fatty acids, eicosapentaenoic acid and docosahexaenoic acid, have positive effects against to cardiovascular diseases. This work was carried out to investigate the fatty acid composition of the most popular fish from Turkey (mainly Istanbul area) and their nutritive values. Total lipid amounts and fatty acid compositions of 6 commonly consumed fish species were determined. Analyses of fatty acid methyl esters were performed by capillary gas chromatography. Palmitic acid (C16:0) and oleic acid (C18:1ω9) were the predominant saturated and monoenoic fatty acids. The predominant polyunsaturated fatty acids were eicosapentaenoic acid (C20:5ω3) and docosahexaenoic acid (C22:6Ω3). European anchovy and European pilchard are concluded to be good dietary sources of ω3-polyunsaturated fatty acids, which are known to reduce the risk of cardiovascular diseases because of their high C20:5ω3 and C22:6ω3 content.     

水酶法提取斑点叉尾鮰内脏油的工艺研究

为提高鱼类加工废弃物的综合利用率,以斑点叉尾鮰内脏为原料,采用水酶法制备鱼油。结果表明：水酶法提取鱼油的最佳工艺条件为初始pH7.5、料液比1:1、加酶量3500U/g、酶解温度55℃、酶解时间0.5h,该条件下鱼油的提取率达到80.94%;提取到的鱼油(即粗鱼油)外观呈黄褐色,具有鱼腥味和轻微的酸败味,其过氧化值较低,而酸值相对较高;粗鱼油中的饱和脂肪酸相对含量为19.42%,单不饱和脂肪酸和多不饱和脂肪酸分别为61.76% 和16.83%,Σn-3/Σn-6 的脂肪酸比值达到3.63。表明斑点叉尾鮰内脏是生产鱼油的良好来源。     

不同提取方式下小黄鱼下脚料粗鱼油脂肪酸组成及挥发性风味成分的变化

为提高小黄鱼下脚料的高值化利用，研究以小黄鱼下脚料为试材，将其进行前处理分别制成湿样（Wet Sample，W）和干样（Dry Sample，D），采用索氏提取法（Soxhlet Extractor Method，S）及酶解法[碱性蛋白酶（1）、中性蛋白酶（2）、木瓜蛋白酶（3）]提取粗鱼油，对其理化指标进行评价、并分析其脂肪酸组成及挥发性风味成分。结果表明，7种不同提取方式（DS、D1、D2、D3、W1、W2、W3）制备的粗鱼油其理化指标值均满足水产标准（SC/T 3502-2016）三级的规定。所得粗鱼油中棕榈酸（C16:0）、硬脂酸（C18:0）、棕榈油酸（C16:1）、油酸（C18:1n9）均为主要脂肪酸，其中D1处理组粗鱼油EPA和DHA相对含量最高，为25.59%。不同提取方式所提粗鱼油中共检出99种挥发性风味成分，包括醇类16种、醛类16种、酮类15种、酯类3种、酸类8种、碳氢化合物16种、酰胺类化合物3种、杂环化合物及其他22种，其中DS处理组粗鱼油的风味与酶解法相比较差，表明冷冻干燥前处理在一定程度上改善了粗鱼油的风味。综上，采用冷冻干燥前处理结合酶解法对小黄鱼下脚料进行提取，提取得到的粗鱼油的品质优良，就其脂肪酸组成而言，多不饱和脂肪酸含量较高，因此其营养价值较高，且该处理有效改善了粗鱼油的风味，可为小黄鱼下脚料的高值化利用提供一定的理论依据与参考。     

Supercritical fluid extraction of fish oil from fish by-products: A comparison with other extraction methods

Fish and fish by-products are the main natural source of omega-3 polyunsaturated fatty acids, especially EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid), both of them with a great importance in the food and pharmaceutical industries. Comparing to conventional fish oil extraction processes such as cold extraction, wet reduction or enzymatic extraction, supercritical fluid extraction with carbon dioxide under moderate conditions (25 MPa and 313 K) may be useful for reducing fish oil oxidation, especially when fish oil is rich in omega-3 such as salmon oil, and the amount of certain impurities, such as some species of arsenic. Furthermore, taking profit of the advantages of supercritical carbon dioxide as extractive solvent, a coupled extraction-fractionation process is proposed as a way to remove free fatty acids and improve fish oil quality, alternatively to physical and chemical refining procedures.     

酶法制备n-3多不饱和脂肪酸型磷脂的工艺

研究了无溶剂体系中固定化磷脂酶A1催化大豆磷脂与乙酯型鱼油进行酯交换反应,制备n-3多不饱和脂肪酸型磷脂的工艺。考察了反应温度、反应时间、底物比(乙酯型鱼油与磷脂的质量比)以及加水量的影响,得到了较优的反应条件。实验结果表明,加酶量(按大豆磷脂的质量计算)20%,底物比8∶1,底物总质量5.0g,加水量55μL,55℃反应12h时,所得产物中EPA和DHA的含量分别为8.0%和17.8%。     

Effects of dietary corn oil and fish oil concentrate on lipid composition of calf tissues

Lipid composition of calf blood plasma, liver platelets, muscle, heart, and brain was measured, as affected by high dietary intake of linoleic acid from corn oil or of polyunsaturated fatty acids from fish oil concentrate. Plasma total lipids, phosphatidylcholine, and cholesteryl esters were reduced by corn oil and fish oil concentrate. Dietary fatty acid composition had no influence on percentage distribution of the major phospholipid components of liver, heart, muscle, and brain, but did alter the polyunsaturated fatty acid composition of major phospholipids in plasma, liver, platelets, muscle, and heart. In general, high linoleic acid intake increased linoleic acid and decreased oleic, arachidonic, and linolenic acids in tissue phospholipids, and fish oil concentrate high in eicosapentaenoic and docosahexaenoic acids increased phospholipid concentrations of these fatty acids. The fatty acid composition of brain phosphatidylcholine and phosphatidyl-ethanolamine was relatively resistant to dietary lipid alterations. The fatty acid changes in tissue phospholipids that resulted from dietary lipid alterations may have important implications in eicosanoid metabolism, and in the structure and function of cell membranes.     

利用微藻培养生产多不饱和脂肪酸研究进展

多不饱和脂肪酸(PUFA),尤其是二十碳五烯酸(EPA)和二十二碳六烯酸(DHA)在营养和医学领域有着重要作用。目前PUFA主要从鱼油中提取,工艺复杂,价格昂贵。微藻中含有丰富的多不饱和脂肪酸,利用微藻生产多不饱和脂肪酸具有广阔的前景。本文综述了微藻培养生产PUFA的研究进展,包括生理作用、合成途径、来源分布及培养方式等。     

Compositional Information Useful for Authentication of Krill Oil and the Detection of Adulterants

Nuclear magnetic resonance (NMR) spectroscopy and chromatography, particularly thin layer chromatography with flame ionisation detector (TLC-FID), were used to investigate fish oil adulteration of krill oil with ethyl esters and triacylglycerol. Natural krill oil has higher levels of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) in phospholipid than in triacylglycerol and so high levels of these omega-3 fatty acids in krill oil triacylglycerol was indicative of adulteration. Carbon (¹³C) NMR detected adulteration of krill oil with 10% or more anchovy oil, while TLC-FID detected levels as low as 1% adulteration with EPA ethyl esters. However, positional distribution of EPA and DHA, as determined using ¹³C NMR, was similar for both fish oil and krill oil, indicating that positional distribution cannot be used to show adulteration. Phosphorous (³¹P) NMR spectroscopy can show adulteration with low cost sources of phospholipid but was not useful for determining adulteration of krill oil with fish oil.     

Manipulation of fatty acid composition of Nile tilapia (Oreochromis niloticus) fillets with flaxseed oil

Nile tilapia (Oreochromis niloticus) is one of the most consumed species among freshwater fish reared in Brazil. However, studies show low levels of n‐3 fatty acids in freshwater fish reared in captivity in comparison with those reared in their natural habitats. The Nile tilapia used in this study were raised in captivity for a period of 5 months and fed varying amounts (0, 1.25, 2.5, 3.75 and 5%) of flaxseed oil as a substitute for sunflower oil (control). No significant differences (P > 0.05) in total lipid (TL) content were found between fillets of tilapia fed the different diets. TL analysis of fatty acid methyl esters by capillary gas chromatography revealed a total of 50 components common to all treatments studied. The major fatty acids present were linoleic acid (18:2n‐6), oleic acid (18:1n‐9) and palmitic acid (16:0). All treatments led to significant % increases in α‐linolenic acid (18:3n‐3), eicosapentaenoic acid (20:5n‐3) and docosahexaenoic acid (22:6n‐3). Increases in both total n‐3 fatty acids and total polyunsaturated fatty acids were observed concomitantly with decreases in total n‐6 fatty acids, resulting in increases in n‐3/n‐6 ratio, with increasing level of flaxseed oil in the feed. Thus feed supplementation with flaxseed oil contributed greatly to raising the nutritional lipid value of Nile tilapia fillets. Copyright © 2007 Society of Chemical Industry     

Evaluation of the potential use of discard species for fish silage and assessment of its oils for human consumption

Waste or by-products contains a substantial amount of nutrients. Fish silage is an alternative way for assessment of fish discards and waste generated in the fish processing industries. The aim of the study was to evaluate the potential use of discard species (Equulites klunzingeri, marine fish and Carassius gibelio, freshwater fish) for fish silage and chemical quality of fish oil extracted from fish silages prepared with acid and fermented methods. Lipid quality of fish oils extracted from fish silages with LAB strains was evaluated in terms of thiobarbituric acid (TBA), peroxide value (PV), p-Anisidine (AV), totox values and fatty acid composition. The results showed that PV, TBA, AV and totox values of all extracted fish oils were within the acceptable limits for edible oils. Recovered fish oils from silage contained high level of polyunsaturated fatty acids (PUFAs), especially eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), serving as a source of good quality fish oil for human consumption.     

微波辅助酶法提取青鱼内脏鱼油工艺优化及脂肪酸组成分析

以青鱼内脏为原料,采用微波辅助蛋白酶提取鱼油,研究酶的种类、酶添加量、酶解时间、酶解温度、微波功率、微波处理时间等因素对鱼油提取得率的影响。采用Box-Behnken响应曲面设计法,建立影响因素和鱼油得率之间的回归方程。结果表明:中性蛋白酶为最佳水解酶,微波功率400 W、酶加入量2%、酶解时间2.5 h、酶解温度45℃、微波处理时间15 min为鱼油最佳提取条件,在此条件下鱼油得率为26.26%±0.13%。使用气相色谱法对萃取的青鱼内脏鱼油脂肪酸组成进行定性和定量分析,结果显示饱和脂肪酸有3种,占总脂肪酸含量的22.39%,主要为棕榈酸和硬脂酸;单不饱和脂肪酸有3种,占总脂肪酸含量的40.42%,主要为油酸和棕榈油酸;多不饱和脂肪酸有8种,占总脂肪酸含量的37.19%,主要为亚油酸。     

乙酯型金枪鱼油不同级分子蒸馏过程中脂肪酸含量及挥发性物质变化

乙酯型金枪鱼油是粗鱼油经过多级分子蒸馏后得到的富含多不饱和脂肪酸,无色无味的优质鱼油,在这个过程中发生了一系列变化。利用气相色谱-质谱联用仪、电子鼻、傅里叶变换红外光谱仪检测不同蒸馏组分的金枪鱼油在成分、风味和性质上的变化以及主要的挥发性物质。结果表明:原料鱼油和不同蒸馏组分鱼油中二十二碳六烯酸(docosahexaenoic acid,DHA)和二十碳五烯酸(eicosapentaenoic acid,EPA)的含量呈先增加后下降趋势,其中EPA含量可达31.41%,DHA含量可达74.10%;二级分子蒸馏可以得到DHA、EPA总含量高达84.26%的乙酯型鱼油,而三级、四级、五级蒸馏鱼油中DHA和EPA含量显著下降。电子鼻检测原料鱼油及不同蒸馏组分的鱼油挥发性物质差异显著。不同蒸馏组分的金枪鱼油主体风味物质为己醛、辛醛、庚醛、壬醛、1-辛烯-3-醇、2-十一酮、2-戊基呋喃等,共同赋予其鱼腥、油脂气息、泥土味、脂肪香味、青草味、蘑菇香、蔬菜香味等。红外光谱分析说明了不同级分子蒸馏后得到的金枪鱼油的主要成分含量是有所不同的。不同蒸馏组分的鱼油中一级、二级鱼油脂类成分种类最多,富集效果最好,而三级、四级、五级分子蒸馏富集效果显著下降。     

气相色谱法测定海豹油中EPA、DPA、DHA含量的方法学研究

目的：建立气相色谱检测海豹油中EPA、DPA和DHA的方法。方法：采用氢氧化钾-甲醇酯化法将海豹油中的脂肪酸快速、有效的转化成脂肪酸甲酯,并通过方法学实验验证其可行性。结果：EPA、DPA和DHA甲酯含量在10～2000μg/mL范围内,峰面积与EPA、DPA和DHA甲酯含量呈良好线性关系;加样回收率在96.93%～103.38%之间,相对标准偏差小于2%;结论：该方法可以快速、准确地同时测定EPA、DPA和DHA含量。     

Enzymatic Synthesis of Refined Olive Oil‐Based Structured Lipid Containing Omega ‐3 and ‐6 Fatty Acids for Potential Application in Infant Formula

Structured lipids (SLs) containing palmitic, docosahexaenoic (DHA), and gamma‐linolenic (GLA) acids were produced using refined olive oil, tripalmitin, and ethyl esters of DHA single cell oil and GLA ethyl esters. Immobilized Lipozyme TL IM lipase was used as the biocatalyst. The SLs were characterized for fatty acid profile, triacylglycerol (TAG) molecular species, solid fat content, oxidative stability index, and melting and crystallization profiles and compared to physical blend of substrates, extracted fat from commercial infant formula (IFF), and milk fat. 49.28 mol% of palmitic acid was found at the sn‐2 position of SL TAG and total DHA and GLA composition were 0.73 and 5.00 mol%, respectively. The total oleic acid content was 36.13 mol% which was very close to the 30.49% present in commercial IFF. Comparable solid fat content profiles were also found between SLs and IFF. The SLs produced have potential for use in infant formulas.     

Omega-3 Fatty Acids in Lake Superior Fish

Proximate analysis and fatty acid composition of eight commercially important species of Lake Superior fish were determined. Palmitic acid (C16:0) was the predominant saturated fatty acid, accounting for 68–79% of total saturated acids. Oleic acid (C18:1) was the most abundant monounsaturated fatty acid. Linoleic acid (C18:2), linolenic acid (C18:3), eicosapentaenoic acid (C20:5) and docosahexaenoic acid (C22:6) were the predominant polyunsaturated fatty acids. Brining, smoking and refrigerated storage caused a reduction in total lipid, but only a small loss in n-3 fatty acids. The data revealed that most Lake Superior fish examined were excellent sources of polyunsaturated fatty acids with very high levels of omega-3 (n-3) fatty acids, especially eicosapentaenoic and docosahexaenoic acids.     

Short communication: malic acid does not promote vaccenic acid accumulation in mixed ruminal fluid with fractionated fish oil by a rumen-simulation technique

The objective of this study was to determine whether malic acid could promote the accumulation of vaccenic acid in the rumen. The control diet was composed of a 65:35 ratio of forage to concentrate with 1% (dry matter basis) added fractionated fish oil (rich in docosahexaenoic acid), and treatment diets consisted of the control diet with added malic acid to achieve final concentrations of 10 mM (treatment 1) and 20 mM (treatment 2), respectively. The experiment was conducted with rumen-simulation equipment (Rusitec) consisting of 9 fermenters. Each treatment included 3 fermenters as replicates. After 7 d of incubation, concentrations of vaccenic acid from treatment 1 (4.38% fatty acids) and treatment 2 (4.46% fatty acids) were similar to that of the control treatment (4.51% fatty acids). The disappearance of docosahexaenoic acid was not different among the control, treatment 1, or treatment 2. These data indicated that malic acid did not promote the accumulation of vaccenic acid in ruminal fluid.     

Carp (Cyprinus carpio) oils obtained by fishmeal and ensilage processes: characteristics and lipid profiles

Fish oil is an important source of long-chain ω-3 polyunsaturated fatty acid. The common carp ( Cyprinus carp ) is a major fish species in world aquaculture production. This study aimed towards obtaining carp viscera oil by ensilage and fishmeal processes. Characteristics of crude oils obtained were also compared with oil extracted by Bligh and Dyer methods. Crude oils obtained by the three processes resulted in significant difference ( P  < 0.05) for free fatty acids, peroxide, thiobarbituric acid and Lovibond colour values; however, iodine and saponification values were not significantly affected ( P  > 0.05). Recovery yield of crude oils was approximately 85% in relation to carp viscera oil. Carp crude oils obtained by the ensilage and fishmeal processes resulted in high unsaturated and polyunsaturated fatty acid contents (67.4%), and ω3/ω6 ratios around 1.15. These oils are applicable in fish diets; however, crude oils require refinement for human consumption.     

鱼油脂肪酸乙酯化工艺研究

比较三种不同鱼油原料脂肪酸组成、含量和各项品质指标,选取步鱼油用碱催化法进行乙酯化反应。通过单因素实验和响应面分析,步鱼油乙酯化工艺最优条件为:无水乙醇/鱼油反应物摩尔比为6:1,反应温度为75℃～77℃,反应时间2小时,碱催化剂浓度为0.8N～1.0N,由分子蒸馏得到乙酯化得率为96％。     

新疆4种典型木本油料油脂脂肪酸和甘三酯组成分析

以新疆4种典型的木本油料沙漠果、碧根果、甜杏仁和巴旦木为原料,测定了4种木本油料种仁的粗脂肪含量、水分及挥发物含量,以及4种油脂的脂肪酸和甘三酯组成。结果表明:4种油料种仁的水分及挥发物含量较低,粗脂肪含量较高,为40. 67%～69. 29%;巴旦木油、碧根果油和甜杏仁油不饱和脂肪酸含量均在90%以上,沙漠果油的不饱和脂肪酸含量为73. 85%; 4种油脂的脂肪酸均以油酸为主(48. 04%～80. 16%);巴旦木油、碧根果油和甜杏仁油以三不饱和脂肪酸甘油酯为主,含量为69. 88%～75. 50%,沙漠果油以二不饱和脂肪酸甘油酯为主,含量为48. 50%; 4种油脂甘三酯均以OOO最多,碳原子当量中均以ECN48最高。