蒙旦树脂烃化学组成及结构特征

本文对中国三种蒙旦树脂烃潦浒树脂烃（ＬＨＴ）,寻甸树脂烃（ＸＤＴ）,舒兰树脂烃（ＳＬＴ）进行了ＧＣＭＳ分析,获取了树脂烃中单元化合物的组成和结构。结果表明,在这三种树脂烃中,主要是五环三萜烃类五环三萜烷,五环三萜烯,单环、二环、三环、四环芳构化五环三萜烷以及三环二萜烃类降松脂烷,降松香烷,降海松烷,松香烷,山达松脂烷,单环、二环芳构化三环萜烷。比较三种树脂的总离子色谱图,发现在寻甸蒙旦树脂烃和舒兰树脂烃中,五环二萜的各种化合物是该组分主要化学组成,尤其在舒兰蒙旦树脂烃中,具有四环芳构化的萜烷其含量占绝对优势。潦浒蒙旦树脂烃中,三环二萜的各种物质是其重要的化学组成。与此同时,阐述了中国蒙旦蜡精制漂白脱色不完全的原因。     

Pd/C催化松脂分子间氢转移反应的集总动力学

以Pd/C为催化剂,在改进的动力学实验装置上研究了松脂分子间氢转移反应的集总动力学.在消除内、外扩散影响的条件下,在线跟踪反应产物并用气相色谱法测定反应体系组成随时间的变化,构造了Pd/C催化剂上松脂分子间氢转移集总反应网络,建立了包含单萜烯、枞酸型树脂酸、海松酸型树脂酸、对伞花烃、氢化单萜烯、脱氢枞酸、氢化枞酸型树脂酸和氢化海松酸型树脂酸等复杂反应体系的集总动力学模型,并估算了模型参数.松脂单萜烯和树脂酸的反应级数分别为1和2,并得到了松脂分子间氢转移中各反应过程的活化能.结果表明,所建动力学模型与实验数据吻合良好,并能预测反应在533 K下的集总组分浓度分布.Pd/C催化松脂分子间氢转移反应以脱氢反应为主,树脂酸的氢转移速率大于单萜烯的氢转移速率.     

云南褐煤蜡氧化精制的研究

本工作对云南潦浒、寻甸、昭通蒙旦蜡进行了脱树脂,氧化精制研究,探索国产蒙旦蜡能否经精制后满足合成改性浅色蜡的要求。实验结果表明,潦浒、寻甸两厂生产的蒙旦蜡经氧化精制不能达到完全脱色,而昭通蒙旦蜡在相同的精制条件下极易脱色,所得浅色蜡质量达到和超过国外同类产品的水平,因此昭通蒙旦蜡是生产浅色蜡的理想原料。在精制反应中,加入适量ＹＰＳＯ－１添加剂,对改善反应条件,产物的分离,提高得率和质量均有良好的影响。文中还讨论了潦浒、寻甸脱脂蜡经氧化精制不能完全脱色的原因     

自制氢化松香主要化学组成的GC-MS法测定

利用自行改进的DEAE－Sephadex离子交换色谱从以玉米松香为原料制备的氢化松香中分离出主要化学组成部分－酸性部分，然后采用DB－5毛细管柱和GC－MS技术对酸性部分进行定性和相对含量测定；共鉴定出6种二氢枞酸型树脂酸，4种二氢海松酸／异海松酸型树脂酸，1种四氢枞酸型树脂酸，2种四氢海松酸／异海松酸型树脂酸；其主要成分为13－二氢枞酸、8－二氢枞酸、13β－7－二氢枞酸、8α，13β－四氢枞酸及8（14）－二氢海松酸等。     

株洲氢化松香主要化学组成的分析

 利用改进的DEAE Sephadex离子交换色谱从株洲氢化松香中分离出主要化学组成部分 酸性部分 ,然后采用DB 5毛细管柱对酸性部分进行气相色谱 质谱 计算机联用分析。共鉴定出 6种二氢枞酸型树脂酸 ,4种二氢海松酸 /异海松酸型树脂酸 ,4种四氢枞酸型树脂酸。其主要成分为 8 二氢枞酸、18 四氢枞酸、13 二氢枞酸、8α ,13β 四氢枞酸、13β 8 二氢枞酸及 8 二氢异海松酸等。     

松香催化加氢过程中树脂酸组成变化的跟踪分析

利用自行改进的DEAE-Sephadex离子交换色谱和气相色谱-质谱-计算机联用(GC-MS-DS)技术研究了在Raney Ni 存在下脂松香催化加氢反应过程中各类树脂酸组成的变化。证实在本实验条件下松香催化加氢过程中的主体反应是树脂酸的二氢化,只伴随少量的四氢化和极少量的脱氢反应。发现在二氢海松酸/异海松酸型树脂酸的分子间存在因双键移位而引起的异构现象。在整个跟踪分析过程中,共检出7种二氢枞酸型树脂酸、5种二氢海松酸/异海松酸型树脂酸及3种四氢树脂酸。     

松脂的催化歧化反应产物的气相色谱-质谱分析

采用气相色谱-质谱技术对松脂的催化歧化新工艺的反应产物进行分析,共分离出45个峰,鉴定出其中的38个化合物,并发现松脂歧化产物中歧化松节油的主要成分为对伞花烃,含量为16.26%;歧化松香的主要成分为脱氢枞酸和氢化树脂酸,其含量分别为41.58%和21.43%。在此基础上对松脂歧化反应过程进行了初步探讨,认为松脂原料中的酸性物质发生分子间氢转移反应,萜烯烃的存在促进了脱氢反应的进行;在树脂酸提供的酸性环境下松脂原料中中性油的主要成分双环单萜烯发生开环异构形成单环单萜烯,单环单萜烯再进行催化脱氢转化为对伞花烃。分析结果表明,直接以松脂为原料进行催化歧化反应可同时获得特级歧化松香和高含量的对伞花烃。     

蒙旦树脂化学组成的研究

采用阴离子交换色谱和硅胶－氧化铝柱色谱对云南寻甸蒙旦树脂（ＸＤＳＺ）、潦浒蒙旦树脂（ＬＨＳＺ）、昭通蒙旦树脂（ＺＴＳＺ）和吉林舒兰蒙旦树脂（ＳＬＳＺ）进行了族组分的分离。树脂游离酸，树脂结合酸，树脂烃和树脂醇在各树脂中的百分含量分别为ＸＤＳＺ１１．８６，８．７６，１２．３０，４５．９９；ＬＨＳＺ１５．８９，１３．９１，４．９０，４５．９９；ＳＬＳＺ２５．４６，８．０７，１７．４０，３６．２２；ＺＴ     

松香树脂酸乙烯酯的研究 第二报:松香树脂酸乙烯酯组成与结构的研究

本文研究了国产特级松香树脂酸乙烯酯的组成与各级分的分子结构：结果表明国产特级松香树脂酸乙烯酯的主要成分是枞酸乙烯酯、长叶松酸乙烯酯和去氢枞酸乙烯酯，三者间重量比为11：3：2；其连接在羧基上的乙烯基在核磁共振谱图中呈现为很好的ABX系统。     

以Pd/C为催化剂的松香加氢反应机理

松香是由松树分泌的松脂经蒸馏而得,其主要成分为枞酸型树脂酸(C19H29COOH)[1]。由于枞酸型树脂酸含有共轭双键,易与大气中的氧作用,使松香的颜色加深、质变脆、热稳定性差、品级下降。松香经催化加氢反应,改变了枞酸型树脂酸的双键结构,使其趋于脂环的稳定结构,消除了松香因共     

舒兰褐煤树脂组分中某些分离物的化学研究

我国褐煤资源丰富 ,分布于云南、吉林、黑龙江、山东和内蒙古等地。褐煤除作燃料和腐植肥料外 ,还应用于轻化工和机械工业 ,如从褐煤制取褐煤蜡。褐煤蜡中含有较多的树脂物质 ,影响了褐煤蜡的质量 ,因此通常褐煤蜡树脂作为废弃物脱除 ,以提高褐煤蜡的质量。褐煤蜡的化学组成为纯蜡和树脂 ,前者为高碳脂肪酸和脂肪醇的酯类、游离脂肪酸和脂肪醇 ,以及烃类物等 ;后者则以萜类为主 ,并含有甾醇、羟基酸和烃化合物[1～ 5] 。 1982年唐运千等采用红外光谱和氢核磁共振谱检定 ,褐煤树脂中含有 β 谷甾醇 ;柱层析和薄层层析检出雌二醇和雌酚酮[2 ] …     

煤酸异构化制对苯二甲酸

进行了煤氧化产物煤酸（水溶酸WSA）钾在催化剂碳酸镉的存在下，异构化制对苯二甲酸(TPA)的研究。主要考察了催化剂用量、二氧化碳初压、反应温度和反应时间对TPA产率的影响。结果表明，在催化剂存在下煤酸可以转化成TPA。单独煤酸钾异构化时，较佳反应条件：温度430 ℃～450 ℃，压力4.0 MPa，催化剂CdCO3用量4%，反应时间2 h。煤酸钾与苯甲酸（BA）钾混合异构化时，较佳反应条件与单独煤酸钾时基本相同。单独煤酸钾在较佳条件下异构化时，粗TPA产率达34%左右，相当于根据其中有效成分苯多羧酸（BPCA）计算的理论产率的75%左右，选择性较好。煤酸钾加苯甲酸钾在较佳条件下异构化时,粗TPA产率可达68%，扣除假定BA自身岐化生成TPA理论产量之后，则煤酸的TPA产率高达70%，比煤酸单独异构化TPA产率(34%)高1倍。粗TPA经精制可得纯度99%以上的精TPA。     

褐煤蜡树脂中多环芳烃组成的研究

采用气相色谱法对云南寻甸褐煤蜡树脂和吉林舒兰褐煤蜡树脂,进行了多环芳烃分布特征的研究,从树脂中鉴定出６８个化合物的同系物。两个树脂样均以菲系化合物占有优势,舒兰树脂中菲系列量约三倍于寻甸树脂的相应量     

褐煤蜡中树脂组分的化学研究：生物标志化合物

用气相色谱－质谱联用仪对吉林舒兰褐煤蜡树脂和云南寻甸褐煤蜡树脂,进行了生物标志化合物的研究。结果指出,三萜类化合物中含有四环三萜、五环三萜、芳香五环三萜和含氧化合物,其中以Ｃ２５Ａ,Ｂ,Ｃ,Ｄ环－四芳鸟散烷和Ｃ２５Ａ,Ｂ,Ｃ,Ｄ环－四芳奥利烷含量最高,舒兰树脂中这两种化合物的含量高于寻甸树脂约１０倍;无羁萜和３－氧代别桦木烷量亦以舒兰树脂占优势     

Development and application of an analytical method for the determination of storage lipids, fatty acids and fatty alcohols in Calanus finmarchicus

A method was developed for the determination of the major storage lipids, wax ester and triglycerides, in the copepod Calanus finmarchicus. A variation of the Folch method was used to extract the lipid. The method was scaled down to enable the extraction of either pooled (-1 mg) or individual (approximately 200 microg) copepods. The major lipid classes were identified using TLC and quantified using HPLC coupled with evaporative light scattering detection. Analysis of laboratory reference materials indicated that this method underestimated the minor triglyceride component, but gave a good estimate of the major wax ester component. The fatty acid and fatty alcohol composition of the C. finmarchicus were determined following trans-esterification of the lipid extract in methanol. Fatty acids and fatty alcohols were initially identified by comparison with authentic standard and by mass spectroscopy. Using GC with flame ionisation detection the normalised area percentage of the fatty alcohols and fatty acid methyl esters was determined simultaneously in one run for either pooled or individual copepod samples. These methods were applied to C. finmarchicus collected from the Irminger Sea, North Atlantic in 2001 and 2002.     

Analytical Characterization of Fatty Acids Composition of Datura alba Seed Oil by Gas Chromatography Mass Spectrometry

Methyl ester derivatives of fatty acids were analyzed for the determination of the constituents of Datura alba seed oil. Gas chromatography coupled to mass spectrometer was used for these analyses. Results delivered that there were saturated as well as unsaturated fatty acids in Datura alba seed oil. Total of 15 different fatty acid components were identified and quantified. Methyl linoleate was found in highest concentration (16.22%) among the identified analytes of interest. In addition methyl esters of Palmitic acid (6.59%), Oleic acid (5.41%) and Stearic acid (1.35%) were found. Concentrations of rest of the detected fatty acids were less than 1%. From the literature it appears that no such work has been performed for the determination of fatty acids in Datura alba seed oil.     

Natural wax constituents of a supercritical fluid CO<Subscript>2</Subscript> extract from quince (<Emphasis Type="Italic">Cydonia oblonga</Emphasis> Mill.) pomace

The chemical constituents of a lipophilic extract from quince (Cydonia oblonga Mill.), obtained by supercritical fluid CO₂ extraction of the dried fruit pomace were investigated. Solvent partition of quince wax with n-hexane or acetone yielded an insoluble (crystalline) and a soluble (oily) fraction. Both fractions were analyzed separately using gas chromatography/mass spectrometry (GC/MS). The insoluble fraction consisted of saturated n-aldehydes, n-alcohols and free n-alkanoic acids of carbon chain lengths between 22 and 32, with carbon chain lengths of 26 and 28 dominating. Also odd-numbered unbranched hydrocarbons, mainly C27, C29 and C31, were detected particularly in the acetone-insoluble fraction (total, 15.8%). By means of vacuum liquid chromatography, triterpenoic acids were separated from the hexane-insoluble matter and identified as a mixture of ursolic, oleanolic and betulinic acids. The major constituents of the hexane-soluble fraction were glycerides of linoleic [Δ^9,12, 18:2] and oleic [Δ⁹, 18:1] acids, accompanied by free linoleic, oleic and palmitic acids (C16). Moreover β-sitosterol, Δ⁵-avenasterol as well as trace amounts of other sterols were assigned. Finally the carotenoids phytoene and phytofluene were identified and quantified by UV/vis and high-performance liquid chromatography/MS techniques, yielding 1.0 and 0.3% of the quince wax, respectively. It is anticipated that the complex of lipid constituents from quince wax may exert interesting biological activities, the elucidation of which awaits further studies. Figure Quince fruits and some of their fruit wax constituents. Clockwise (starting at one o’clock): structure formulas of Δ5-avenasterol, linoleic acid, oleanolic acid, and phytofluen. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Investigation of Fatty Acid Composition of Ammi majus Seed Oil by Gas Chromatography Mass Spectrometry

The Ammi majus seeds oil constituents of methyl ester derivatives of fatty acids were analyzed using Gas Chromatography coupled to mass spectrometer. The results obtained containing the saturated as well as unsaturated fatty acids of majus seeds oils. A total of 18 different components were identified and quantified. Methyl ester of linoleic acid was found in high concentration 9.00%, among the identified analytes of interest. In addition methyl ester of Oleic acid 5.60%, Palmitic acid 3.98% Linolenic acids 1.42% were found. Concentration of the rest of identified fatty acids analytes were less than 1%. Thus from the results it is apparent that due to the presence of high percentage of valuable analytes concentrations detected in the fatty acid of A. majus, has increased its importance for the consumption in the pharmaceuticals as well as its applications in the new formulations for various skin diseases to prevent and cure from different infections.