Composition of neutral fractions in Chinese raw tall oil

Chinese tall oil samples, obtained from pulp and papermaking factories in Qinzhou and Jiamusi of China, were first divided into acidic and neutral fractions by saponification, extraction, and distillation. The obtained neutral fractions were then analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) after silylation with bis-(trimethylsilyl) trifluoroacetamide. The results obtained show that 10 types of compound (monoterpenes, sesquiterpenes, diterpenes, triterpenes, resin alcohols, resin aldehydes, steroids, fatty alcohols, phenols, stilbenes) exist in the neutral fractions of Chinese raw tall oil. In the neutral fractions from Qinzhou, 55 components were identified, 35 of which were found for the first time in Chinese raw tall oil; 12 components were discovered for the first time in raw tall oil. In the neutral fraction from Jiamusi, 45 components were identified, 9 of which were discovered for the first time in Chinese raw tall oil.     

酚羟基保护法合成硬脂酰单宁酸酯及其抗氧化性能评价

为解决单宁酸(TA)亲水性强亲油性弱的问题,以单宁酸为原料,利用苄基溴将单宁酸的部分酚羟基保护后得到单宁酸苄基醚(TBE),再以硬脂酸酐为酰基化试剂,吡啶为催化剂,N_2保护下反应,引入长链脂肪烃;最后在弱酸条件下将苄基水解脱去,制得硬脂酰单宁酸酯(C_(18)-TA)。采用均匀实验优化合成条件,傅里叶红外光谱(FT-IR)、紫外光谱(UV)、核磁共振(~1H NMR)表征了C_(18)-TA的结构,并通过C_(18)-TA清除·DPPH的能力和抗油脂氧化能力评价其抗氧化性能。结果表明:优化最佳合成条件为单宁酸1 g,硬脂酸0.6 g,吡啶1.5 mL,反应温度80℃,回流时间265 min,得到的C_(18)-TA产率可达87.98%。使用酚羟基保护法制得的C_(18)-TA不仅改善了单宁酸的表面活性,而且保留了单宁酸中多数的酚羟基,抗氧化能力明显高于单宁酸和丁基羟基茴香醚(BHA),质量浓度为0.05~0.25 g/L,对·DPPH的清除率为91.96%~97.39%;对亚麻籽油的抗氧化值(POV)升高缓慢,0~30 d为3.82~17.72 mmol/kg。     

芍药种子含油率与脂肪酸成分研究

[目的]本文对芍药种子含油率、脂肪酸成分及含量进行了探讨,为芍药开发成油料植物提供参考。[方法]选取芍药36个栽培品种和1个野生居群为样本,采用索氏提取法提取种子油脂并测定含油率,用气相色谱—质谱联用仪(GC-MS)对提取的籽油成分进行分析。[结果]表明:芍药36个栽培品种和1个野生居群种子平均含油率为20.20%。芍药籽油主要含有豆蔻酸、棕榈酸、棕榈一烯酸、硬脂酸、油酸、亚油酸、亚麻酸和花生酸8种脂肪酸,其中,亚麻酸含量最高,平均达34.14%,其次为油酸和亚油酸,这3种不饱和脂肪酸的含量占全部脂肪酸的93.37%。芍药籽油脂肪酸含量变化相对稳定,各脂肪酸成分的变异系数从大到小依次为亚油酸(13.90%)油酸(13.51%)亚麻酸(10.71%)棕榈酸(0.18%)硬脂酸(0.09%)花生酸(0.002%)、棕榈一烯酸(0.002%)豆蔻酸(0.00%)。[结论]芍药种子含油率高,富含亚麻酸、亚油酸和油酸,且含量相对稳定,变异很小,具有开发为高含量亚麻酸食用油潜力。     

油桐种籽油脂合成及其在品种类型上的差异

油桐种籽成熟过程中,种籽的含油量和水分含量是负相关。水分的亏缺,严重影响了油脂合成。从 8月 25日至 9月 15日含油量上升23.8％,而含水量下降24.55％,桐酸含量也上升,与此同时棕榈酸、硬脂酸、油酸、亚油酸以及亚麻酸的含量下降。桐酸在总脂肪酸含量中占79.42％。脂肪酸的累积、转化最活跃时期在8月份和9月上旬,这时期油桐栽培水分供应是至关重要的。 油桐不同种和品种(类型)脂肪酸组成有明显差异,以桐酸变化幅度最大,差值达16.06％。在这些样品中,桐酸含量超过76％的有15份,均为三年桐,其中少花单生果品种(类型)占12份,千年桐桐酸含量均不到70％。从油质来说,三年桐优于千年桐。在三年桐中少花单生果品种(类型)具有桐酸含量高,亚油酸、油酸含量较低的优点。     

Components of the essential oils of Azadirachta indica A. Juss, Azadirachta siamensis Velton, and Azadirachta excelsa (Jack) Jacobs and their comparison

The components of the essential oils from seeds of Azadirachta indica, Azadirachta siamensis, and Azadi-rachta excelsa were studied by gas chromatography and gas chromatography-mass spectrometry. The main components of A. indica oil were hexadecanoic acid (34.0%), oleic acid (15.7%), 5,6-dihydro-2,4,6-triethyl-(4H)-1,3,5-dithiazine (11.7%), methyl oleate (3.8%), and eudesm-7(11)-en-4-ol (2.7%). The major components of A. siamensis oil were hexadecanoic acid (52.2%), tricosane (10.5%), tetradecanoic acid (6.8%), oleic acid (4.9%), and pentacosane (4.9%). Azadirachta excelsa oil contained oleic acid (31.3%), hexadecanoic acid (14.2%), octadecanoic acid (13.0%), 4-octylphenol (9.7%), and O-methyloximedecanal (6.8%) as the main constituents. The essential oils from A. indica, A. siamensis, and A. excelsa were found to contain fatty acids (52.6%–72.3%) as major components. The minor components of the oils were n-alkanes, aromatics, esters, sulfur and nitrogen compounds, and terpenoids. Differences in oil composition were observed between the three species.     

圆齿野鸦椿籽油提取工艺及脂肪酸组分分析

为高效利用圆齿野鸦椿籽油,采用正己烷加热回流提取圆齿野鸦椿籽油,分别考察了提取时间、提取温度和正己烷-圆齿野鸦椿籽粉末比(液料比)对圆齿野鸦椿籽油提取得率的影响。以单因素试验的结果为依据,运用Design-Expert 8.0.6软件进行Box-Behnken响应面设计及数据分析,进一步对回流提取圆齿野鸦椿籽油的工艺进行优化。研究结果表明:各因素影响提取得率的主次顺序为提取时间、提取温度、液料比;最佳提取工艺是加热回流提取时间62.04 min,提取温度80.2℃,液料比10.14∶1(mL∶g),该条件下提取得率的预测值为5.84%,通过验证实验发现,提取得率实验值为(5.85±0.001)%,与预测值接近,两者的相对误差为0.17%,说明响应面优化的圆齿野鸦椿籽油提取工艺稳定、可行。同时,对圆齿野鸦椿籽不同部位提取得到的油脂进行分析,种仁出油率为(35.6±0.7)%,种皮出油率为(2.1±0.15)%,对籽油成分进行分析,检测出18种脂肪酸成分,其中不饱和脂肪酸达到65.52%,亚油酸的量最高,达45.64%。     

REFINING OF SULFATE SOAP AND EXTRACTING OF PHYTOSTEROLS

The sulfate soap Is refined through extracting unsaponlfiablc neutral substan比usingethyla以tatc and hcxanc—acctonc.The contentofncutralsubstancelntallolldccreasesfrom32.8％to 7.4％and 18％The acid number oftalloilincrcascsfrom！19to！69and！53Thequalityoftall oil Is greatly improved.ThlSprovides a favorable condition for distillation of tall oil.Theunsaponlfiablc neutral substancenom crude sulfate soap mainly consists of tcrPCnc aldchydcs,Icrpcnc alcohols,fatty alcohols and sterols Inwhlch larlxol Is 26.3％and 18.5％;sterols arc 17％and 27.l％M paratcly.The wb！to crystals containing sterols of96.9％are obtalncdbycrystalhaatlonand rccrystalllzatlon The sterols arc mainly g一sltostcrol and campcsterol.     

不同产地油茶籽油脂肪酸组成研究

运用气相色谱技术分析了河南、湖北、湖南及广西地区产茶籽油脂肪酸的组成。结果表明:茶籽油中油酸、亚油酸、亚麻酸含量及不饱和脂肪酸总含量与产地纬度有关。其中,油酸、亚麻酸含量及不饱和脂肪酸总含量随产地纬度的降低呈现出升高的趋势,而亚油酸的含量随产地纬度的降低呈现出先降低后升高的趋势。     

栝楼籽油的理化性质及其脂肪酸组成分析

采用索式提取器萃取栝楼籽油,经甲酯化处理后,用气质联用仪（GC-MS）对栝楼籽仁油的脂肪酸组成进行分析和鉴定,面积归一法计算各种成分的质量分数,并对其理化性质进行分析研究。结果表明：从栝楼籽仁油中捡出19种脂肪酸：10种饱和脂肪酸,以棕榈酸、硬脂酸为主,占脂肪酸总量8．019％;9种不饱扣脂肪酸,以油酸、亚油酸和栝楼酸为主,占总量的91．603％。理化测定结果表明：栝楼籽的出仁率为55．8％,种仁含油率为51．4％,折光指数为1．4831,皂化价为190．2mg KOH／g,碘价为120．9gI2／100g,酸价为1．62mgKOH／g,过氧化值为0．85meq／kg,可见栝楼籽油是一种值得开发利用的营养保健油源。     

圆锥梾木种仁油理化性质及脂肪酸成分分析

采用索氏抽提法提取圆锥梾木种仁油,分析了种仁油理化指标,并利用气相色谱质谱联用技术(GC-MS)对油的脂肪酸组成进行了分析。结果表明:圆锥梾木种仁出油率为7.0%,折光指数为1.4804,相对密度0.98,酸值(KOH)39.46mg/g,皂化值(KOH)175.94mg/g。经GC-MS分析鉴定,圆锥梾木种仁油检出11种脂肪酸成分,检出率99.70%。其中,饱和脂肪酸4种,含量占比为7.51%,不饱和脂肪酸7种,含量占比92.19%,未知成分0.3%。     

木质纤维成分的乙酸分离方法及表征

研究了一种用含有少量硫酸的乙酸溶液分离杨木成分的方法。考察了反应时间、乙酸浓度、液比和催化剂浓度对木材成分分离的影响。对分离出的木材三种成分进行了表征。结果表明,分离杨木成分的较佳条件为:硫酸浓度0.3%,液比6,反应时间3h和乙酸浓度90%。残渣的主要成分是α-纤维素和半纤维素。水不溶沉淀物(乙酰化木质素)的重均分子量分布在341到253之间,分散性系数分布在1.1到1.2这一窄范围内。糖分析结果表明,可溶性成分主要来源于半纤维素,以单糖形式存在。     

韦塔桉叶片脂肪酸的提取及成分的GC-MS分析

以丙酮为提取溶剂,物料粒度为100~200目,料液比1:15,浸泡8 h,萃取时间为1.5 h,在超声功率为80 khz,30℃时对韦塔桉桉叶油进行提取,并用GC-MS对其成分进行分析。结果得到韦塔桉桉叶油的提取率为19.04%,经GC-MS分析得到韦塔桉桉叶油含有10种脂肪酸,其中亚油酸和亚麻酸为不饱和脂肪酸。桉叶油中棕榈酸、亚油酸、亚麻酸及硬脂酸的绝对含量分别为0.82%、0.86%、0.15%、0.33%,占提取粗脂总量的2.16%。     

Synthesis of new betaine-type amphoteric surfactants from tall oil fatty acid

Two new betaine-type amphoteric surfactants — betaineN,N'-dihydroxyethyl-N-ethyl fatty acid ester and ammoniumN-(fatty acid ester) ethyl-N,N-bis (2-hydroxyethyl)-3-(2-hydroxypropyl) sulfonate — were synthesized using tall oil fatty acids as the raw materials. Processing conditions suitable for synthesizing the intermediates and final products were probed. In addition, the chemical structures of the intermediates and the final products were identified by infrared spectroscopy, hydrogen nuclear magnetic resonance spectroscopy, and elemental analysis.     

Investigations on tall oil of Southern Pine wood

The residue from tall oil distillation, known as tall oil pitch (TOP), was investigated by GC/MS analysis. Several separation techniques such as preparative TLC and extractions from solutions of different pH were applied. Apart from about 4% distilled free acids (fatty and diterpenoid) and 5% steroids (sitosterol and sitostadiene) two new fatty acids C-26 and C-28 could be detected. About 1% of lignin like material could be isolated after continuous extraction with chloroform.The authors wish to express their gratitude to the Österreichische Nationalbank for financially supporting the purchase of the gas chromatographic equipment. The authors also thank Dr. A. Nikiforov for providing the mass spectroscopical equipment     

橡胶籽油ω-3脂肪酸的富集工艺参数及品质判定研究

对橡胶籽毛油及富集后成分、含量的测定,观察不同富集工艺参数和油源品质的优劣,试验结果:尿素包合法最佳工艺条件为温度30℃、包合反应时间12h、尿素和脂肪酸比例为3.0∶1(m∶m);新鲜橡胶籽油中ω-3脂肪酸含量为20.74%,包合后可达39.91%。B-820型脂肪酸测定仪测定的精度高,重现性好,易操作,适用于测定脂肪酸成分及含量。     

雪岭云杉针叶叶绿素—胡萝卜素软膏酸性物质化学组成的研究

雪岭云杉针叶叶绿素－胡萝卜素软膏中含酸性物质约２２％（占软膏重）,其中脂肪酸占４４．８６％,树脂酸占５２．４９％。该酸性物质经气相色谱和质谱定性,定量分析,共分离出３１个峰,鉴定出２６个化合物,被的组分占酸性物质总量的９７．３５％。其中主要成分为检酸（２１．５５％）,异海松酸（１２．８９％）、油酸（１２．０７％）、亚麻酸（７．３１％）、新纵酸（６．１０％）等。研究发现,雪岭云杉针叶叶绿素－胡萝卜素     

Synthesis of 1-hydroxyethyl-2-alkyl-2-imidazoline and its derivative sulfonate amphoteric surfactant from tall oil fatty acid

1-Hydroxyethyl-2-alkyl-2-imidazoline (HEAI) and its derivative sulfonate amphoteric surfactant were synthesized using tall oil fatty acid as the raw material. Suitable experimental conditions for synthesizing the intermediate and final products were probed. Their chemical structures were also investigated by means of infrared spectroscopy and hydrogen nuclear magnetic resonance spectroscopy. Based on the results of these analyses, it has been found that during the reaction process of HEAI with sodium 3-chloro-2-hydroxypropane sulfonate under alkaline condition the imidazoline ring was hydrolyzed to amides, and the obtained amphoteric surfactant was actually a complex mixture of amides. An etherification reaction in the hydroxyethyl group was also observed when the HEAI/sodium 3-chloro-2-hydroxypropane sulfonate molar ratio was more than 1:1.     

中国五针松组松脂的化学特征

本文研究了中国五针松组松脂的化学特征。从中分离出糖松酸(Lambertianicacid),其含量高达9.7％～25.0％,并经IR、MS、NMR、UV、旋光度及元素分析等鉴定。这种双萜酸在国内属首次分离和鉴定。同时,在红松、新疆五针松和大别山五针松松脂中又鉴定出一定数量的松柏烯(Cembrene),这在中国松属松脂中也属首次发现。     

不同基肥对油用牡丹结籽性及籽脂肪酸组分的影响

【目的】为给南方地区油用牡丹高效栽培种植技术的完善提供理论参考,以四川湿润气候区的油用牡丹‘凤丹’品种为研究对象,比较了不同基肥的施用对牡丹结实情况和籽脂肪酸组分及含量的影响。【方法】共设置了油枯(0.1、0.5 kg/株)、牛粪(0.1、0.5 kg/株)、牛粪(0.1、0.5 kg/株)+复合肥(0.1 kg/株)6个基肥处理,观测不同基肥处理下油用牡丹结籽性,采用索氏抽提法测定油用牡丹籽粗脂肪含量,采用气相质谱法(CG-MS)对油用牡丹籽单体脂肪酸进行定性定量分析。【结果】在单株施牛粪0.1 kg+复合肥处理下,油用牡丹的单籽质量(0.470±0.029) g,籽长(10.452±0.266) mm,籽宽(8.660±0.056) mm,均好于其他施肥处理。油用牡丹籽粗脂肪含量在不同基肥处理下差异不明显,但单体脂肪酸含量存在显著差异。经GC-MS分析,在油用牡丹籽油中检测出13种单体脂肪酸,其中有8种饱和脂肪酸(癸酸、月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、花生酸、榆树酸和木蜡酸),3种单不饱和脂肪酸(棕榈烯酸、油酸和顺-11-二十碳烯酸),2种多不饱和脂肪酸(亚油酸和亚麻酸);其中亚麻酸的含量最高(40.27%),其次为亚油酸和油酸,分别为29.02%、22.03%。【结论】单株施牛粪0.5 kg+复合肥处理对促进油用牡丹籽亚麻酸含量提高的效果最佳,在该处理下亚麻酸含量可达(45.97±0.01)%。