Py－GC－MS和LC－MS技术在褐煤结构研究中的应用

摘要Ｄａｍｓｔｅ等用快速热阵气相色谱和快速热解气相色谱－质谱法（Ｐｙ－ＧＣ－ＭＳ）对西班牙的五种褐煤进行了分子结构研究。用该项技术，使煤中大分子有机结构在惰性气氛中降解，形成的化合物在线分离，鉴定和定量分析，得到了用其它方法难以取得的较详细的煤大分子结构信息。Ｂｏｎｎｅｔｔ等借助流动带界面液相色谱－质谱法（ＬＣ－ＭＳ）对煤中卟啉同系物进行了分离和鉴定。此法可证明Ｃ＿（３２），Ｃ＿（３１），Ｃ＿（３０）和Ｃ＿（２９）多烷基卟啉在劣质褐煤抽提物离析出的血红素馏分中以配位体形式存在。     

高效微型液相色谱与高温气相色谱联合测定润滑油族组成

采用填充毛细管液相色谱（ＰＣ－ＨＰＬＣ）与高温毛细管气相色谱（ＣＧＣ）在线联用技术分析润滑全组分。ＰＣ－ＨＰＬＣ柱用于样品族分离（烷烃、单环芳烃、双环芳烃１三环芳烃与胶质）经ＰＣ－ＨＰＬＣ分离后的各族组分被依次存放在多位储存接口内,然后分别转入ＧＣ作单个族组分的定量分析。该方法是解剖进口润滑油基础油及新产品开发中强有力的分析手段。     

HNO3氧化褐煤制取黄腐酸

用硝酸氧化寻甸褐煤制得氧化褐煤，用含水１０％的丙酮萃取黄腐酸。考察了ＨＮＯ_３浓度、氧化时间及煤酸比对黄腐酸收率的影响。对氧化褐煤和黄腐酸进行了工业分析和总腐植酸、游离腐植酸、总酸性基、羧基、酚羟基的测定。结果表明，褐煤经硝酸氧化可大大提高黄腐酸的收率，是生产农用抗旱剂及工业、医药用黄腐酸的有效途径。     

Py—GC—MS和LC—MS技术在褐煤结构研究中的应用

Ｄａｍｓｔｅ等用快速热解－气相色谱和快速热解气相色谱－质谱法对西班牙的五种褐煤进行了分子结构研究。用该项技术，使煤中大分子有机结构在惰性气氛中降解，形成的化合物在线分离，鉴定和定量分析，得到了用其它方法难以取得的较详细的煤大分子结构信息。Ｂｏｎｎｅｔｔ等借助流动带界面液相色谱－质谱法对煤中卟啉同系物进行了分离和鉴定。此法可证明Ｃ３２，Ｃ３１，Ｃ３０和Ｃ２９多烷基卟啉在劣质褐煤抽提物离析出的血红素馏     

褐煤对碱性染料吸附的研究

褐煤对碱性染料阳离子黄Ｘ－８ＧＬ单组分水溶液的吸附，在平衡浓度较低时，比较好地符合Ｌａｎｇｍｕｉｒ和Ｆｒｅｕｎｄｌｉｃｈ吸附平衡等温线。其吸附速率主要受染料分子在吸附剂粒子内部扩散的影响。褐煤对碱性染料具有很强的吸附能力，平衡溶液化学耗氧量（ＣＯＤ）值较低。     

Ca—Si处理钢用MgO—C质浸入式水口

文中对开发出的Ｃａ－Ｓｉ处理钢用ＭｇＯ－Ｃ材质与原来的ＡＧ材质进行了比较，ＭｇＯ－Ｃ材料的耐蚀性优于ＡＧ材质，Ｃａ－Ｓｉ处理钢用浸入式水口采用ＭｇＯ－Ｃ材质，其抗氧化和耐蚀性有明显的效果。     

NGC－818鞋用胶粘剂

ＮＧＣ－８１８鞋用胶粘剂本品是经接枝改性的氯丁胶粘剂，主要用于制鞋业上。１９９３年３月通过技术鉴定，其性能达到国内先进水平。１．主要技术内容本品含ＮＧＣ－Ａ、ＮＧＣ－Ｂ、ＮＧＣ－Ｃ、ＮＧＣ－Ｄ四个牌号，它们不仅具有耐水、耐酸、耐碱的性能，而且对各种材...     

从褐煤中提腊

云南寻甸化工厂、潦浒化工厂、云南勘探设计院、北京煤化所、太原燃化所等单位,贯彻执行“自力更生”方针,互相协作,在燃化部和省、市的直接领导与关怀下,从一九六九年开始,发展了从褐煤中提腊的科研工作,取得了一定成果。潦浒、寻甸两地现已建成褐煤提腊工厂,并于一九七一年试车。褐煤腊又称“蒙旦腊”,是褐煤(或泥煤)经有机溶剂萃取而得的萃取物,为粗褐煤腊,氧化脱色可得各种浅色褐煤腊。褐煤腊主要用在:电缆工业,导火索、炸药防潮、电气制品脱模剂、各种上光腊、     

大口径毛细管GC与GC／MS测定50%辛—氰乳油

本文报道大口径毛细管ＧＣ与ＧＣ／ＭＳ对辛－氰乳油中辛硫磷鉴定和氰戊菊酯进行定量分析的改进方法。用ＧＣ－９Ａ气相色谱仪。ＦＩＤ检测器，甲基硅酮柱并采用程序升温，ＱＰ－５０００ＧＣ／ＭＳ对辛硫磷鉴定，辛硫磷在本实验条件下稳定。本方法因收率为９９．２１－１００．４９％。变异系数为０．６２－１．６６％，现行检测辛－氰乳油方法（ＨＰＬＣ分析辛硫磷，ＧＣ法分析氰戊菊酯）比较二进无显著性差异，但成本低，操作简单     

CH－12型石蜡加氢精制催化剂研制及工业应用

ＣＨ－１２型石蜡加氢精制催化剂以改性国产载体Ｃ负载Ｗ－Ｍ－Ｍ活性组分，呈三叶草外形，具有良好的抗破碎强度、活性稳定性和芳烃炮和能力．适宜的加氢脱硫与加氢脱氮性能．使产品食品级石蜡具有良好的光安定性，含油量不变，稠环芳烃饱和良好。工业催化剂制备流程与工艺条件可行，催化剂产品质量稳定。     

Biological activities of the rice bran extract and physical characteristics of its entrapment in niosomes by supercritical carbon dioxide fluid

The objectives of this study were to compare the biological activities of the rice bran (Oryza sativa Linn.) extracts prepared by supercritical carbon dioxide fluid (scCO₂) and ethanolic maceration, and the physical properties of niosomes entrapped with the extracts prepared by scCO₂ and chloroform film method. The scCO₂ extract showed higher unsaturated fatty acid and phenolic contents than the maceration extract. All extracts showed no significant difference of biological activities. The characteristics of niosomes entrapped and not entrapped with the extract prepared by scCO₂ and chloroform film method were not different with a unilamellar nano-sized structure and the phase transition temperatures at 80 °C. The gradual decrease trend of the vesicular membrane microviscosity with less membrane rigidity at higher extract concentrations was observed. The scCO₂ technique is advantageous for the preparation of the rice bran extracts and niosomes because of no requirement of organic solvents and having less step.     

Photooxidation of Nimbin and Salannin, Tetranortriterpenoids from the Neem Tree (Azadirachta indica)

Nimbin and salannin, major triterpenoids accompanying azadirachtin in extracts of neem (Azadirachta indica) seeds, were photooxidized by UV light in the presence of oxygen to more polar, unstable intermediates that rearranged on silica gel to two final products in which the furan ring had been oxidized to isomeric hydroxybutenolides. The isomeric hydroxybutenolides were also readily formed when a crude extract of triterpenoids from neem seeds was irradiated, and both isomers of salannin have been isolated from seeds. Photooxidation of nimbin and salannin proceeded much faster than that of azadirachtin. All photoproducts showed some biological activity againstSpodoptera littoralis, Locusta migratoria, andSchistocerca gregaria. Isonimbinolide was as potent as azadirachtin at inhibiting feeding in all three species, and it also inhibited the growth ofS. littoralis. Isosalanninolide showed potent antifeedant and growth inhibitory activity againstS. littoralis.     

Olfactory basis of cannibalism in grasshoppers (Orthoptera: Acrididae): II. field assessment of attractants

The responses of rangeland grasshoppers to biologically and historically derived attractants were studied in a shortgrass prairie in southeastern Wyoming in July 1990. Seven long-chain fatty acids (C₁₄–C₂₀: singly and in combination), grasshopper cadavers, molasses, fruit extracts, and chloroform (solvent control) were tested. Each attractant was applied to filter paper and placed in an arena delimited by a 0.10-m² aluminum ring. Grasshoppers were most attracted to linoleic and linolenic acids, with significantly more grasshoppers found in these arenas than in those of the controls or other attractants. These two fatty acids alone and in combination were more attractive at 1 grasshopper equivalent (GE) than at 5 GE. The seed bug,Lygaeus kalmii Stål, and five species of ants were also attracted to these two fatty acids. Molasses had significantly more grasshoppers on the filter paper than did the other attractants, but molasses had significantly fewer grasshoppers in the arena than the fatty acids. Fruit extracts were not effective at attracting grasshoppers. Water extracts of cadavers attracted significantly more grasshoppers to the bait than did chloroform extracts. Because the assayed grasshopper community was dominated by the Gomphocerinae (a subfamily that includes many pest species that do not readily consume wheat bran bait), it may be possible to use fatty acids in conjunction with insecticidal bran baits for increased control of rangeland grasshoppers.     

5-溴代胡椒环的合成方法研究

以胡椒环为原料,采用氧化溴化体系合成5-溴代胡椒环,确定了溴化工艺条件,考察了溶剂种类、反应温度、物料配比及反应时间对反应的影响。优化工艺为:三氯甲烷为反应溶剂,反应温度为10℃,反应时间为6 h,物料配比n(胡椒环)∶n(氢溴酸)=1∶1.2。产品收率81%,产品纯度99.5%(GC)。产物的结构经1H NMR、IR、MS表征。     

Application of non-reductive alkylation in liquid ammonia to studies on macromolecular structure of coals and bitumen-derived asphaltene

The reaction of non-reductive ethylation of a coal anion generated in the presence of a strong base (sodium and/or potassium amides) in liquid ammonia is an efficient method for coal solubilization. Under the reaction conditions used, over 50 wt % of vitrinites separated from carboniferous bituminous coals became soluble in chloroform. The chloroform extracts were characterized by relatively low molecular weights ranging from 600 to 12000. At the same time, Athabasca oil sand asphaltene, which, under reductive conditions, degrades relatively easily to lower molecular weight species, did not display any molecular weight changes on reacting with amides in liquid ammonia. This fact stresses the non-destructive character of non-reductive alkylation. It appears, therefore, that the molecular weights of chloroform soluble portions of ethylated vitrinites reflect the molecular size of the original vitrinites. These results contradict the concept of coal having a highly crosslinked macro-molecular structure.     

阴香叶提取物的抑菌活性初步研究

用不同溶剂对阴香[Cinnamomum burmanii (Nees) Bl] 叶进行提取,以生长速率法测定了提取物对植物病原真菌的抑菌作用。结果表明:阴香叶的氯仿提取物的抑菌活性最好;氯仿提取物对西瓜枯萎菌、芒果炭疽菌、香蕉枯萎菌和香蕉炭疽菌的EC50分别是0.3193mg/ml、0.1552mg/ml、0.0226mg/ml、0.019 2 mg/ml,其中提取物对香蕉炭疽菌的毒力最高,值得进一步研究。     

厚果鸡血藤提取物对两种同翅目害虫的生物活性

测定了厚果鸡血藤种子和根提取物对褐飞虱和桃蚜两种同翅目害虫的生物活性,结果表明,它们对这两种害虫有很高的触杀活性,对桃蚜有一定的胃毒活性。用不同溶剂提取时,三氯甲烷提取物的活性明显高于甲醇提取物的活性。用相同溶剂提取时,种子提取物的活性比根提取物活性高。对褐飞虱、桃蚜的触杀活性及对桃蚜的胃毒活性均以种子三氯甲烷提取物最高,种子三氯甲烷提取物对褐飞虱、桃蚜的接触LD50值分别为0.25、0.03g/头,对桃蚜的胃毒LC50值为1342mg/L。四种提取物对两种害虫的毒力顺序为:种子三氯甲烷提取物>根三氯甲烷提取物>种子甲醇提取物>根甲醇提取物。     

Glandular Trichome Extracts from Medicago sativa Deter Settling by the Potato Leafhopper Empoasca fabae

Extracts of glandular trichomes from Medicago sativa were tested for their ability to disrupt the settling behavior of the potato leafhopper, Empoasca fabae. Erect and procumbent glandular trichomes were mechanically isolated from stem sections of resistant genotype "G98A," and nonglandular trichomes were collected from susceptible cultivar "Ranger." Isolated trichomes were extracted with chloroform, acetone, and ethanol, and the resulting crude extracts were applied to the surface of a sachet containing an artificial diet. Leafhoppers were offered a two-way choice between crude trichome extracts from G98A and Ranger. All three of G98A solvent extracts caused various degrees of diet rejection, resulting in the crude Ranger trichome extracts being preferred over G98A extracts. Overall, the fewest leafhoppers settled on the ethanolic extracts. Additional bioassays documented a dose response associated with G98A ethanolic extracts when compared with Ranger trichome extracts and a solvent control. No difference in preference behavior was detected between Ranger trichome extracts and a solvent control. Gas chromatography-mass spectrometry analysis revealed a homologous series of nonvolatile fatty acid amides C(n)H(2n+1)NO (n = 19-23) unique to G98A glandular trichome extracts.     

Fluorescent pigments from uterus of vitamin E-deficient rats

Spectrophotofluorometric analyses of the extracts of uterus from sterile rats maintained on a vitamin E-deficient diet for a prolonged period of time indicated that the brown ceroid-like pigments present were highly fluorescent, having characteristics typical of products formed during lipid peroxidation in vivo. The aqueous-methanol layer of the uteral extract from vitamin E-deficient animals had higher fluorescence than the corresponding chloroform layer, indicating the presence of more polar water-soluble pigments than those found in most other tissues so far examined.     

Bioactive Phytochemicals from Wild Arbutus unedo L. Berries from Different Locations in Portugal: Quantification of Lipophilic Components

The lipophilic composition of wild Arbutus unedo L. berries, collected from six locations in Penacova (center of Portugal), as well as some general chemical parameters, namely total soluble solids, pH, titratable acidity, total phenolic content and antioxidant activity was studied in detail to better understand its potential as a source of bioactive compounds. The chemical composition of the lipophilic extracts, focused on the fatty acids, triterpenoids, sterols, long chain aliphatic alcohols and tocopherols, was investigated by gas chromatography–mass spectrometry (GC–MS) analysis of the dichloromethane extracts. The lipophilic extractives of the ripe A. unedo berries ranged from 0.72% to 1.66% (w/w of dry weight), and consisted mainly of triterpenoids, fatty acids and sterols. Minor amounts of long chain aliphatic alcohols and tocopherols were also identified. Forty-one compounds were identified and among these, ursolic acid, lupeol, α-amyrin, linoleic and α-linolenic acids, and β-sitosterol were highlighted as the major components. To the best of our knowledge the current research study provides the most detailed phytochemical repository for the lipophilic composition of A. unedo, and offers valuable information for future valuation and exploitation of these berries.