溶剂法提取万寿菊籽油的工艺研究

采用3种不同溶剂,运用索氏提取法进行了万寿菊籽油的提取实验研究。首先考察了以工业正己烷为溶剂时回流时间、回流次数对万寿菊籽油提取率的影响,确定了提取率最大时的最佳工艺条件,并与最佳条件下以乙醚和正己烷-乙醚(1∶1)作溶剂时的提取率进行了对比。研究结果表明:以工业正己烷为溶剂时的最佳提取条件是回流时间为7 h、回流次数为14次.h-1,以工业正己烷、乙醚、正己烷-乙醚(1∶1)为溶剂时对应提取率分别为22.53%、23.96%、25.56%。     

怒江漆油中高级脂肪酸成分

对云南怒江漆油 (漆树籽油 )进行皂化得到了漆油的总脂肪酸 ,将总脂肪酸甲酯化得到总脂肪酸甲酯 ,用GC MS联用仪测定了所含高级脂肪酸的成分 ,结果表明云南怒江漆树油中高级脂肪酸分别为棕榈酸、油酸、硬脂酸、花生酸、二十烷二酸。其中 ,棕榈酸的质量分数高达 76.9%。     

迎春花脂肪酸成分的GC/MS分析

采用乙醚提取迎春花脂肪酸,再经过甲酯化后,通过气相色谱/质谱联用技术分析脂肪酸的组成。共检出九种脂肪酸成分,主要成分分别为棕榈酸(29.27%)、亚油酸(19.75%)、二十碳三烯酸(16.63%)和十四(烷)酸(14.69%)。     

青梅醇提物中乙酸乙酯萃取组分的GC-MS分析

青梅醇提物中的抗氧化活性成分主要被乙酸乙酯所萃取.对青梅乙酸乙酯萃取组分进行了GC-MS分析,共检测出24个峰,其中鉴定出14种成分.主要成分为各类有机酸类化合物,约占总量的72.99%,其中含量较高的是柠康酸酐20.31%、6-十八碳烯酸16.58%、顺-油酸12.6%、十六烷酸10.72%、十八烷酸6.17%、癸酸1.97%、辛酸1.33%等.其次是二氢香豆酮7.38%和(2S)-1,3,4,5,6,7-六氢-1,1,5,5-四甲基-2H-2,4a-甲桥萘2.09%.     

云南八角籽油的化学成分研究

以云南富宁八角茴香为原料,以石油醚为溶剂,索氏法提取八角籽油,通过GC-MS分析法对八角籽油进行分析,并用峰面积归一法确定各组分的含量。结果表明,大红八角籽油中反式大茴香脑含量高达68.10%;干枝与角花八角籽油具有高含量的n-棕榈酸(分别为29.70%、29.13%)和大茴香醛(分别为16.62%、9.11%)。可见,不同采摘时期的八角籽油的成分与含量均有很大不同。     

南方红豆杉叶挥发性成分

分别以二氯甲烷和乙醚作溶剂,采用低温冷凝,同时蒸馏萃取南方红豆杉干叶挥发性成分,极性色谱柱(DB-WAX)气-质联机分析。鉴定出63种化合物,主要是脂肪族类(39种),其次为芳香族类(11种),而萜类化合物占比例很小(6种)。按两种萃取溶剂所得分析结果平均值,主要成分是十六烷酸(21.19%)、十四烷酸(8.87%)、亚麻酸乙酯(3.49%)。相比已有的关于南方红豆杉叶油成分分析的报道,新鉴定出己醛、2-己烯醛、1-辛烯-3-醇、2,4-庚二烯醛、苯乙酮等34种有青香、花香、果香香气的微量或痕量低沸点化合物。所鉴定化合物以邻二氯苯为内标定量,总含量为88.16μg/g红豆杉叶。     

小球藻USTB-01脂的提取和转化生物柴油研究

研究了乙醚、正己烷、石油醚、乙酸乙酯、石油醚-乙醚混合溶液(体积比2∶1)和氯仿-甲醇混合溶液(体积比1∶1)分别浸提小球藻USTB-01中油脂的效果,发现石油醚-乙醚混合溶液从小球藻USTB-01细胞中提取脂类的效果最好。在此基础上,探索了研磨、反复冻融、超声波破碎和超声波结合反复冻融这4种不同破壁处理方式对油脂提取率的效应,结果表明采用超声波结合反复冻融法破壁后,与未经任何破壁处理时相比,油脂提取率提高了2.7倍。进一步研究显示,在提取的藻脂中分别加入水、柠檬酸、磷酸、草酸和EDTA进行高温水化脱胶,发现柠檬酸的脱胶效果最好。采用碱催化甲酯化法,将小球藻USTB-01油脂转化为脂肪酸甲脂,经气相色谱质谱测定结果显示,其主要成分为以C16∶0和C18∶1为主的脂肪酸甲酯,为进一步生产高品质生物柴油奠定了重要的基础。     

香樟树籽油提取及其在化妆品中的应用

研究了采用石油醚萃取香樟树籽油脂的制备工艺及其在化妆品中的应用。结果表明,最佳提取条件为:料液比为1∶5(g/mL),反应温度50℃,反应时间2.5 h;香樟树籽油主要脂肪酸有辛酸(0.34%)、癸酸(54.46%)、月桂酸(38.27%)、棕榈酸(0.22%)、硬脂酸(0.07%)、油酸(2.99%)、亚油酸(0.31%),其中癸酸甘油三酯、月桂酸甘油三酯93%以上;用香樟树籽油脂取代白油和单甘脂应用于保湿霜化妆品中,与其他组分相容性较好,保湿效果增强,各项理化指标达到或超过国家标准。     

25%稻瘟净-杀螟松油混合剂的薄层分析

25％稻瘟净和杀螟松混合油剂是由稻瘟净和杀螟松原油和清油、α-甲基苯乙烯等溶剂配制而成的。其中除稻瘟净和杀螟松的有效成分外,还有很多杂质。这些杂质在定量测定时的干扰很难除去。我们在硅胶薄层上,用正己烷∶乙酸乙酯∶乙醚(8∶2∶3)为展开剂,使各欲测成分和所有杂质分离。测定稻瘟净时,刮取R_f≈0.17处的色带,用甲醇提取,用浓硝酸和高氯酸熔化,加入偏钒酸铵和钼酸铵试剂,使成磷钼钒酸黄色溶液。在波长420nm处测定其消光值。     

番荔枝籽油脂脂肪酸组成的GC-MS分析

研究了番荔枝籽油脂中脂肪酸的组成.用索氏脂肪抽提器提取番荔枝籽的油脂,并以GC-MS分析油脂脂肪酸的组成.结果表明,番荔枝籽油脂收率达29.2％;番荔枝籽油脂中含有8种脂肪酸,主要为:油酸(45.37％)、亚油酸(30.68％)、棕榈酸(13.60％)和硬脂酸(8.94％),其中不饱和脂肪酸含量达76.29％.番荔枝籽含油量高,脂肪酸种类丰富,尤其是不饱和脂肪酸含量较高,具有较高的开发利用价值.     

藻类水热液化产物生物油分离纯化及组分分析

杜氏盐藻通过水热液化制备得到的生物油,先采用溶剂分割分别得到正己烷相、二氯甲烷相和乙醚相,再对二氯甲烷相进行柱层析分离纯化。正己烷相和乙醚相直接通过GC-MS和FT-IR进行分析,二氯甲烷相先经柱层析分离后结合GC-MS、二次质谱和FT-IR等确认不同馏分的产物组成。研究结果表明:二氯甲烷相经柱层析分离可得到16个馏分,分别是石油醚馏分(A₁),主要是烯烃类;石油醚:乙酸乙酯馏分(A₂),主要是酸类化合物;石油醚:丙酮馏分(A₃),主要是酰胺类;石油醚:甲醇馏分(A₄),主要是烷烃类;甲醇馏分(A₅),主要是十八碳烯酰胺。经柱层析分离纯化后,生物油的回收率高达91.38%;获取较全的生物油组分信息,为藻类液化机理的分析和生物油的改质提供了依据。     

Soybean oil microemulsions with oleic acid/glycols as cosurfactants

The preparation of biocompatible microemulsions of soybean oil in systems made of anionic surfactant, oleic acid, water, and several glycols was considered. The selected glycols were ether derivatives (methyl, ethyl, dimethyl, and diethyl ether) of ethylene glycol and diethylene glycol. The study was performed using pseudoternary phase diagrams in which the three apexes were occupied by soybean oil, a combination of surfactant/oleic acid, and a combination of water/glycol, respectively. The widest regions of microemulsions were obtained for systems containing methyl ether and especially ethyl ether of both ethylene glycol and diethylene glycol. The two latter compounds allowed the preparation of oil-in-water, bicontinuous, and water-in-oil microemulsions with final surfactant contents of 3–4%.     

Minor components responsible for flavor reversion of soybean oil

Edible refined, bleached and deodorized (RBD) soybean oil was fractionated by silicic acid column chromatography to identify minor components responsible for flavor reversion. Minor components from oil eluted with diethyl ether/n-hexane (1:1) were compared with those from corn and canola oils. All vegetable oils contain free fatty acids, diglycerides and sterols as major ingredients in this fraction. However, unusual triglycerides consisting of 10-oxo-8-octadecenoic acid and 10-and 9-hydroxy octadecanoic acids were detected in RBD and crude soybean oils.     

乙酸仲丁酯在山茶油提取中的应用研究

在食品安全性要求日渐严格的背景下,文章使用不含硫和芳烃的绿色环保溶剂乙酸仲丁酯替代植物油抽提溶剂,实现了山茶油的提取。通过对各影响因素进行系统研究,获得了乙酸仲丁酯作抽提溶剂的最佳工艺参数:温度50℃,3∶1的溶剂比,提取时间为1 h,在该优化条件下的出油率可达到96.7%,明显优于同等条件下的乙酸乙酯、石油醚(60~90℃)、正己烷和乙醇。经简单的减压蒸馏分离回收溶剂,其溶剂残留率为11%,仅比正己烷高出4%。乙酸仲丁酯用以取代植物油抽提溶剂将具有可行性。     

A study on fatty acids in seeds of Euterpe oleracea Mart seeds

Fatty acids of Euterpe oleracea Mart seeds were analyzed in hexane and diethyl ether extracts. The hexane extract contained dodecanoic acid (3), tetradecanoic acid (4), hexadecanoic acid (7), and 9-octadecenoic acid (10). The diethyl ether extract contained (10). The oil of Mart seeds was obtained firstly by methanol extract and further extracted with diethyl ether. The hexane and diethyl ether extracts were then analyzed for antioxidant effects. Both extracts demonstrated a 1,1-diphenyl-2-picrylhydrazyl radical elimination effect similar to that of α-tocopherol and an active oxygen inhibition effect. Significant quantities (0.6212 mg/mL) of polyphenol, in comparison to the standard rejected gallic acid, were found in the extract oil of Mart seeds by the methanol extraction.     

Concentrated solutions of SBS block copolymers in solvent mixtures

The viscosities of 10% and 20% solutions of linear and non-linear SBS block copolymers were measured in various solvent pairs comprising ethyl acetate/toluene, ethyl acetate/cyclohexane, ethylacetate/carbon tetrachloride, ethyl acetate/n-hexane, ethyl acetate/cyclohexanone, methyl ethyl ketone/cyclohexanone and methyl ethyl ketone/n-hexane. Addition of the second solvents to 10% solutions of the polymers in ethyl acetate or methyl ethyl ketone gave rise to peaks around 10% to 14% added solvents. These peaks are caused by phase separation involving micelles and their occurrence depends on the interplay of composition of solvent mixtures, molecular weight and solution concentration and not on polymer architecture, styrene content or state of shear.     

用氨基钠还原剂合成香料乙基柏木醚

柏木醚是柏木醇的脂肪族醚。由柏木油中提取的柏木醇３２ｇ、１７６ｍｌ二甲苯、氨基钠７ｇ，在１１５～１２５℃下回流２ｈ，冷却，慢慢滴加３２ｇ硫酸二乙酯，在１１５～１２５℃回流１ｈ，分馏，在１１３～１１４℃／０．１６ｋＰａ下收集乙基柏木醚，产率８９％，含量９６％。     

ACEI系列药物前手性中间体2-氧代-4-苯基丁酸的合成

探索了用苯甲醛为起始原料合成普利系列血管紧张素转换酶抑制剂(ACEI)药物的前手性中间体2 氧代 4 苯基丁酸(OPBA)的全流程。由苯甲醛与醋酸酐在无水醋酸钾催化下缩合制得肉桂酸、加氢得到苯丙酸、乙酯化后获得苯丙酸乙酯,以苯丙酸乙酯与草酸二乙酯经缩合反应生成中间体3 苄基 2 氧代丁二酸二乙酯,然后经w(H2SO4)=15%的稀硫酸水解制得目标产物OPBA。用正交实验法对合成OPBA的关键步骤苯丙酸乙酯与草酸二乙酯的缩合-水解反应进行了综合优化,得到适宜合成条件为:n(苯丙酸乙酯)∶n(草酸二乙酯)=1∶3;反应温度60℃;缩合时间1 5h;水解时间15h,OPBA产率65%。     

Fractionation of commercial frying oil samples using sep-pak cartridges

Commercial frying oil samples were fractionated by column chromatography on hydrated silicic acid according to the standardized DGF-IUPAC-AOAC method. The non-polar fraction was isolated using a mixture of petroleum ether:diethyl ether (87:13), while the polar fraction was eluted by diethyl ether. These used frying oil samples were also fractionated using Sep-Pak cartridges. The non-polar fraction was eluted with 20 ml of a mixture of petroleum ether:diethyl ether (92:8), while the polar fraction was eluted with methanol. The purity of each fraction was studied by thin layer chromatography (TLC) and by the Iatroscan TLC/FID system using a mixture of hexane:tetrahydrofuran:acetic acid (97:3:1) as solvent system. The Sep-Pak and the standardized methods gave similar results. This indicates that the state of degradation of a frying oil (detection of polar components) could be studied using Sep-Pak cartridges, which is less time- and solvent-consuming than column chromatography.     

Fatty Acid Profile and Bioactive Compound Extraction in Purple Viper's Bugloss Seed Oil Extracted with Green Solvents

Oil extraction from seeds of purple viper's bugloss (Echium plantagineum) was carried out using different solvents (chloroform:methanol, n-hexane, ethanol, 2-propanol and ethyl acetate) at room temperature and also using Randall extraction. Extraction yields were calculated and oils were analyzed in terms of fatty acid profiles and distribution among lipid classes, total polyphenol content, oxygen radical absorbance capacity (ORAC) and phytosterol content. No considerable differences were found on fatty acid profiles and distribution in oils regardless of the solvent and temperature used for the extraction. However, ethanol combined with Randall extraction (85 °C for 1 hour) offered the best results in terms of total polyphenol content (20.9 mg GAE/100 g oil), ORAC (468.0 μmol TE/100 g oil), and phytosterol amount (437.2 mg identified phytosterols/100 g oil) among all assayed extraction methods. A higher extraction temperature led to significantly higher concentrations of bioactive compounds and ORAC values in the oil when ethanol or 2-propanol were used as extracting solvent, but that was not the case using n-hexane except for the concentrations of β-sitosterol and stigmasterol, which were significantly higher using Randall extraction than room temperature extraction with n-hexane. Ethanol is classified as a “green solvent,” and it could be considered a suitable option to produce oil from E. plantagineum seeds with a higher antioxidant capacity and bioactive compound concentration than the current commercial oil, which is usually extracted with n-hexane.