气相色谱法测定鱼油中的二十碳五烯酸、 二十二碳六烯酸和二十二碳五烯酸

目的通过优化鱼油中二十碳五烯酸(eicosapentaenoic acid,EPA)、二十二碳六烯酸(docosahexaenoic acid,DHA)和二十二碳五烯酸(docosapentaenoic acid,DPA)的测定条件,建立鱼油中EPA、DHA和DPA气相色谱定量检测分析方法。方法采用正己烷处理样品,经色谱柱(Agilent,Elite-WAX,30 m×0.25 mm,0.25μm)分离鱼油中的EPA、DHA、DPA甲酯标准品,并进行定量检测。结果 EPA浓度在0.36~3.6 mg/m L、DHA浓度在0.37~3.7 mg/m L、DPA浓度在0.16~1.62 mg/m L的范围内与峰面积的线性良好,相关系数r0.999。在80%、100%、120%添加水平下,EPA、DHA和DPA的检出限分别为0.01%、0.03%、0.009%,EPA、DHA和DPA的回收率分别为96.2%、96.4%、95.7%。结论气相色谱法灵敏度高、准确、重现性好,适用于鱼油中EPA、DHA和DPA的含量测定。     

气相色谱法多重检验海豹油中二十碳五烯酸、 二十二碳五烯酸和二十二碳六烯酸方法研究

目的建立多重检验海豹油中二十碳五烯酸(eicosapentaenoic acid,EPA)、二十二碳五烯酸(docosapentenoic acid,DPA)和二十二碳六烯酸(docosahexaenoic acid,DHA)的气相色谱法。方法用氢氧化钾甲醇溶液将样品中EPA、DPA和DHA甲酯化,气相色谱程序升温同时分析3个ω-3多不饱和脂肪酸,分别用外标法和内标法进行定量。结果 3个ω-3多不饱和脂肪酸的外标法定量线性范围为50~5000μg/m L,相关系数均0.999,精密度相对标准偏差均10%,回收率均90%;内标法定量的精密度相对标准偏差均10%,回收率均85%;外标法和内标法对3个ω-3多不饱和脂肪酸的结果比较,CV%均小于10%。结论该方法操作简单快捷,适用于进口海豹油中EPA、DPA和DHA的含量简便和准确的测定。     

气相色谱法测定鱼油软胶囊中二十碳五烯酸和 二十二碳六烯酸的柱前衍生化方法改进

目的建立柱前衍生-气相色谱法测定保健食品中二十碳五烯酸(eicosapentaenoic acid,EPA)和二十二碳六烯酸(docosahexaenoic acid,DHA)含量的分析方法。方法鱼油软胶囊经皂化后用1%的硫酸-甲醇甲酯化,用气相色谱法测定,FID检测器检测,色谱柱为DB-FFAP(30 m×0.25 mm,0.25μm),进样口温度250℃,检测器温度260℃,柱温215℃,直接进样,外标法定量。结果 EPA和DHA在0.05~5 mg/mL范围内线性良好(r_(EPA)=0.9999,r_(DHA)=0.9999),EPA和DHA的回收率分别为93.1%~102.3%和92.2%~103.9%,EPA和DHA的相对标准偏差均小于3%。结论该方法操作简便、快捷,避免了有毒试剂的使用,定量准确,重现性好,适合大批量样品的快速检测。     

DHA软胶囊中3种特征标志物的测定及其品质评价

针对不同来源的DHA软胶囊,建立一种同时测定其3种特征标志物的检测方法,并结合其他理化指标进行品质的综合评价。建立的特征标志物测定方法为:样品经甲酯化衍生化处理后,采用外标法对不同DHA软胶囊中DHA、EPA、亚油酸的甲酯进行检测,脂肪酸甲酯经换算得到相应脂肪酸的含量。4个品牌的产品性状、酸价、过氧化值、砷均符合国家相关标准。特征标志物测定的方法学验证结果为:DHA甲酯、EPA甲酯及亚油酸甲酯的精密度RSD分别为1.39%、1.43%、0.5%;线性范围分别为0.3~2.4 mg/mL、0.2~2.4 mg/mL、0.1~1.6 mg/mL,相关系数分别为1.000、0.999 9、1.000,线性关系均良好;平均回收率分别为96.9%~101.4%、97.5%~100.3%、95.4%~99.6%,准确度较高;定量限浓度分别为0.08、0.04、0.03 mg/mL;24 h内的稳定性数据(RSD)分别为3.19%、3.65%、3.02%,说明稳定性好。DHA软胶囊的评价结果表明:3#的酸价较高,崩解较慢;2#的DHA和亚油酸含量较低;0#DHA软胶囊的亚油酸含量明显高于其他品牌。与其他理化指标相比,3种特征标志物在4个品牌产品之间差异较明显,可较好地反应关键品质变化。     

乙酰氯-甲醇甲酯化法测定婴幼儿配方乳粉中脂肪酸含量方法的优化

目的改进乙酰氯-甲醇甲酯化气相色谱(gas chromatography,GC)法测定婴幼儿配方乳粉中脂肪酸含量的方法。方法改进了乙酰氯-甲醇配制的体积浓度,考察了不同甲酯化反应温度和时间对月桂酸、肉豆范酸、亚油酸(linoleic acid,LA)、α-亚麻酸(α-linolenic acid,α-LA)、二十二碳六烯酸(docosahexaenoic acid,DHA)和花生四烯酸(arachidonic acid,AA)含量测定的影响,并验证了改进方法的检出限、重现性和回收率等。结果采用改进的乙酰氯-甲醇配制液可将甲酯化反应时间缩短至60 min,在4℃下保存该配制液有效期达10 d。各组分在一定质量浓度范围内线性关系良好(r>0.999)。改进方法中月桂酸、肉豆蔻酸、亚油酸、α-亚麻酸、二十二碳六烯酸和花生四烯酸的检出限为0.11~0.68 mg/100 g,定量限为3.3~20.4 mg/kg,与国标方法相比定量限提升了38.2%~95.0%,回收率均在95%~105%之间,稳定性相对标准偏差为0.79%~2.59%。结论改进方法能满足婴幼儿配方乳粉中脂肪酸含量的检测。     

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。     

乳品中5种脂肪酸的测定

建立了气相色谱法同时测定奶粉中亚油酸、α-亚麻酸、花生四烯酸、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)的高通量分析方法。简化奶粉中提取脂肪的方法,改进脂肪酸甲酯化方法。采用三氟化硼甲醇法衍生,5种脂肪酸的线性范围为25～5 000 mg/L,样品的亚油酸在0.05,0.1和0.2 g/g(脂肪)3个水平的添加回收率为84.9%～109.0%之间,相对标准偏差为2.0%～11.0%;α-亚麻酸在10,20和30 mg/g(脂肪)3个水平的添加回收率为81.5%～122.3%之间,相对标准偏差为3.9%～9.2%;花生四烯酸、二十碳五烯酸(EPA)、二十二碳六烯酸(DHA)在1,2和3 mg/g(脂肪)3个水平的添加回收率为61%～119%之间,相对标准偏差为2.0%～9.5%;方法的定量限为25μg/g脂肪。方法简便、快速、准确,适用于奶粉中5种脂肪酸的测定。     

气相色谱法同时检测南极磷虾中2种ω-3脂肪酸含量

目的 建立使用甲酯化-气相色谱法同时检测南极磷虾中二十碳五烯酸(eicosapentaenoic acid, EPA)和二十二碳六烯酸(docosahexaenoic acid, DHA)含量的分析方法。方法 样品经二氯甲烷提取后,与0.5%硫酸-甲醇溶液在60 ℃条件下反应30 min,反应液使用硅酸镁柱层析净化。将洗脱液转移至15 mL离心管中,2000 r/min离心20 min,上清液氮吹浓缩后,用乙腈定容至1 mL,使用DB-1701色谱柱(30 m × 0.32 mm, 1.00 μm)分离,火焰离子化检测器检测,外标法定量。 结果 方法在0.02~2.00 mg/mL的线性范围内,相关系数大于0.9999。扣除水分的影响,同一部位的新鲜、干燥样品相对偏差小于10%;平行样品的相对标准偏差不超过6%（n = 3）,平均回收率大于82.6%。结论 该方法简便高效,检出限低、重现性好,可用于新鲜和冻干南极磷虾样品中EPA和DHA的检测。     

利用脂肪酶制取富含多不饱和脂肪酸油方法

<正>1 前言 我们知道,共轭亚油酸(CLA)、α-亚麻酸(ALA)、γ-亚麻酸(GLA)、双高γ-亚麻酸(DGLA)、花生四烯酸(AA)、二十碳五烯酸(EPA)、二十二碳五烯酸(DPA)、二十二碳六烯酸(DHA)等各种多不饱和脂肪酸(PUFA)对人体具有各种不同生理活性,因国内外已有许多论文阐述,不再赘述。     

毛细管气相色谱内标法同时测定奶粉中亚麻酸、ARA、EPA和DHA

建立了以二十一烷酸甲酯为内标物,同时测定奶粉中亚麻酸ARA、EPA和DHA的毛细管气相色谱方法。试样经氢氧化钾-甲醇甲酯化后、生成相应的脂肪酸甲酯,再经气相色谱分析、内标法定量。结果表明,奶粉中亚麻酸、ARA、EPA、DHA和内标物均获得良好的分离;4种被测组分色谱峰面积与其质量浓度有良好线性关系,相关系数均大于0.998;样品加标回收率为95.4%～104.7%,变异系数为2.168%～4.368%,检出限为1.0mg/100 g。该方法操作简便、快速、准确,适合批量奶粉中亚麻酸、ARA、EPA和DHA的测定。     

Effects of abomasal infusions of fatty acids and 1-carbon donors on apparent fatty acid digestibility and incorporation into milk fat in cows

Our primary objective was to determine the effects of the abomasal infusion of 16-carbon (16C) and 22-carbon (22C) fatty acids (FA) on apparent FA digestibility, plasma FA concentrations, and their incorporation into milk fat in cows. Our secondary objective was to study the effects of 1-carbon donors choline and l-serine on these variables. Five rumen-cannulated Holstein cows (214 ± 4.9 d in milk; 3.2 ± 1.1 parity) were enrolled in a 5 × 5 Latin square experiment with experimental periods lasting 6 d. Abomasal infusates consisted of (1) palmitic acid (PA; 98% 16:0 of total fat), (2) PA + choline chloride (PA+CC; 50 g/d of choline chloride), (3) PA + l-serine (PA+S; 170 g/d of l-serine), (4) behenic acid (BA; 92% 22:0 of total fat), and (5) docosahexaenoic acid algal oil (DHA; 47.5% DHA of total fat). Emulsions were formulated to provide 301 g/d of total FA and were balanced to provide a minimum of 40 and 19 g/d of 16:0 and glycerol, respectively, to match the content found in the infused algal oil. Apparent digestibility of FA was highest in DHA, intermediate in PA, and lowest in BA. Digestibility of 16C FA was lowest in BA and highest in PA. The digestibility of 22C FA was highest in DHA relative to BA (99 vs. 58%), whereas 1-carbon donors had no effect on 22C FA digestibility. Plasma 16C FA concentrations were greatest with PA treatment, and 22C FA concentrations were ~3-fold greater in DHA-treated cows relative to all other treatments. Milk fat 16:0 content was highest in PA relative to BA and DHA (e.g., 37 vs. 27% in PA and DHA), whereas the milk yield of 16:0 was higher in PA relative to DHA (i.e., 454 vs. 235 g/d). Similarly, milk 22:0 content and yield were ~10-fold higher in BA relative to all other treatments, whereas DHA treatment resulted in higher content and yield of 22:6 in milk fat relative to all other treatments (41- and 38-fold higher, respectively). Consequently, the content of FA >16C (i.e., preformed) was higher in milk fat from cows infused with BA and DHA relative to PA. De novo FA content in milk did not differ between PA, PA+CC, and PA+S (~16% of milk fat) but was higher in BA and DHA treatments (19 and 21%, respectively). We conclude that FA carbon chain length and degree of saturation affected FA digestibility and availability for absorption as well as their incorporation into milk fat. The abomasal infusion of choline chloride and l-serine did not modify these variables relative to infusing palmitic acid alone.     

奶粉脂肪酸与乳制品风味关系研究

用气质（GC—MS）联用色谱分析了11个商业奶粉样品的脂肪酸组成以及含量,每个样品均检测到了28种脂肪酸,在表现奶粉风味的4个呈味脂肪酸,也即辛酸、己酸、壬酸和葵酸中只检测到了辛酸和葵酸。辛酸和葵酸含量在进口奶粉中普遍高于国产奶粉。国产奶粉中辛酸和葵酸的含量以2号最好,3号其次。亚油酸含量在国产奶粉中普遍高于进口奶粉。     

Determination of ethanol,volatile fatty acids,lactic and succinic acids in fermentation liquids by gas chromatography

A rapid and simple quantitative method was developed to determine, by gas chromatography, the concentrations in fermentation liquids of ethanol, the C₂-C₆ volatile fatty acids, and lactic and succinic acids. Aqueous samples were acidified with 250μlml^?1 metaphosphoric acid (5:1 ratio), centrifuged, and injected directly on to a column containing a porous aromatic polymer (Chromosorb 101) maintained at 200°C in a gas chromatograph fitted with a flame ionisation detector. It was unnecessary to purify samples further before injection, although distillation and ion-exchange methods were examined. Derivatisation of lactic and succinic acids before injection was not necessary, but the lowest level of detection of these two relatively non-volatile acids was about four times greater than that for the volatile fatty acids. The method described was suitable for the analysis of rumen fluid, methane digester fluid, silage extracts and other anaerobic fermentation fluids. The relative retention times are given for 23 organic acids and six other fermentation end-products.     

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     

磁化处理对脂肪酸精馏过程的影响

在不同磁感应强度的磁场中,研究了磁化处理对脂肪酸精馏过程的影响。研究结果表明,磁场对脂肪酸的精馏过程有一定的影响,脂肪酸经磁化处理后,油酸的含量提高0.41%～0.64%,收率提高0.30%～0.47%;亚油酸的含量提高0.46%～0.69%,收率提高0.37%～0.54%;硬脂酸的含量提高0.44%～0.62%,收率提高0.34%～0.48%。由此可见,磁化处理有利于脂肪酸精馏过程的进行。     

Effects of addition of malic or citric acids on fermentation quality and chemical characteristics of alfalfa silage

We studied the effects on alfalfa preservation and chemical composition of the addition of different levels of malic acid and citric acid at ensiling as well as the utilization efficiency of these 2 organic acids after fermentation. Alfalfa was harvested at early bloom stage. After wilting to a dry matter content of approximately 40%, the alfalfa was chopped into 1- to 2-cm pieces for ensiling. Four levels (0, 0.1, 0.5, and 1% of fresh weight) of malic acid or citric acid were applied to chopped alfalfa at ensiling with 4 replicates for each treatment, and the treated alfalfa forages were ensiled for 60 d in vacuum-sealed polyethylene bags (dimensions: 200 mm × 300 mm) packed with 200 to 230 g of fresh alfalfa per mini silo and an initial density of 0.534 g/cm³. The application of malic or citric acids at ensiling for 60 d led to lower silage pH than was observed in the control silage (0% of malic or citric acids). Application of the 2 organic acids led to higher lactic acid concentration in alfalfa silage than in the control silage except with the application rate of 1% of fresh weight. Silages treated with both organic acids had lower nonprotein nitrogen concentrations than the control silages, and the nonprotein nitrogen concentrations in ensiled forages decreased with the increase in malic or citric acid application rates. The application of the 2 organic acid additives led to lower saturated fatty acid proportions and higher polyunsaturated fatty acid proportions in ensiled alfalfa than in the control silage. The amount of malic and citric acids degraded during ensiling of alfalfa was 1.45 and 0.63 g, respectively. At the application rate of 0.5% of fresh weight, residues of malic acid and citric acid in alfalfa silage were 11.1 and 13.6 g/kg of dry matter. These results indicate that including malic or citric acids at the ensiling of alfalfa effectively improved silage fermentation quality, limited proteolysis, improved fatty acid composition of the ensiled forage, and could provide animals with additional feed additives proven to promote animal performance. However, when the application rate of both organic acids reached 1%, the concentration of lactic acid in silages decreased notably. Additionally, 0.5 and 1% application rates also increased the yeast count in ensiled alfalfa.     

过氧乙酸灭菌效果及酸残留的实验研究

目的 研究过氧乙酸灭菌的效果及酸的残留量对pH值的影响。方法 用微生物学无菌检测法和pH值测定法。结果 满载,少量装载,重复灭菌时达到无菌效果,△pH均在0.3～0.4之间。结论 经过氧乙酸灭菌的塑料瓶能达到无菌要求,酸的残留量对pH值的影响不显著,生产上可用过氧乙酸灭菌法对不耐热的内包材进行灭菌。     

Growth of Aeromonas hydrophila K144 as Affected by Organic Acids

The influence of different acids on the aerobic growth kinetics of Aeromonas hydrophila was studied in BHI broth with 0.5 and 2.0% NaCl incubated at 5 and 19°C. Growth curve data were analyzed by the Gompertz equation and a nonlinear regression program; generation and lag times were calculated from the Gompertz parameters. Type of acid, pH, NaCl level and temperature influenced lag and generation times. The organic acids (acetic, lactic, citric and tartaric) inhibited growth at higher pH values than inorganic acids (HCl and H₂SO₄). The high NaCl level interacted with type of acid and pH to restrict growth of the organism at the lower temperature of incubation. Acetic and lactic acids were effective in controlling the growth of A. hydrophila and could readily be combined with low holding temperature to render foods free of the organism.     

花生四烯酸、二十二碳六烯酸和二十碳五烯酸 在炎症中的作用概述

心脑血管疾病、肿瘤、糖尿病、神经系统疾病、自身免疫等疾病严重危害着人类的生命和健康,并消耗着大量医疗资源。事实上,很多疾病发生和发展的背后都伴随着炎症反应,炎症是众多疾病的病理基础,甚至是导致这些疾病的诱因。炎症本身是机体的防御性反应,但过度的炎症反应和长期慢性炎症会损害机体的稳态。炎症的调节和控制由炎症介质介导,花生四烯酸(arachidonic acid,AA)、二十二碳六烯酸(docosahexaenoic acid,DHA)和二十碳五烯酸(eicosapentaenoic acid,EPA)等长链多不饱和脂肪酸(10ng-chain polyunsaturated fatty acids,LC-PUFAs)的衍生物是一类重要的调控炎症的介质。炎性细胞间的交流和细胞内信号传递与LC-PUFAs有关。AA经环氧酶和脂氧合酶合成的类二十烷酸主要起促炎作用,但有的也有抗炎作用。DHA和EPA在体内起抗炎作用,由它们合成的消退素(resolvins,Rvs)和保护素(protectin,PD)是重要的抗炎活性物质。DHA和EPA还可以干扰炎性细胞内信号传导途径来抑制炎症反应。本文从炎症与疾病的关系、LC-PUFAs的衍生物及其促炎和抗炎机制等方面综述了AA、DHA和EPA在炎症中的作用。     

杂多酸催化合成辛酸蔗糖酯

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