气相色谱/质谱法分析研究蜂胶中化学成分

1　引　　言用ＧＣ/ＭＳ分析方法分离鉴定蜂胶中的化学成分。试样经提取、酯化、浓缩后 ,采用ＨＰ 5( 30ｍ× 0 .2 5ｍｍ× 0 2 5ｍｍ)弹性石英毛细管柱进行测定。分离鉴定了黄酮类、脂肪酸、芳香酸、醇类等 77个化合物。用峰面积归一法通过Ｇ1 70 1ＢＡ化学工作站数据处理系统得出各化学成分在蜂胶中的百分含量为 97 1 2 %。2　实验部分2 1　仪器与试剂　ＨＰ6890 / 5973ＧＣ/ＭＣ联用仪 (美国惠普公司 ) ,三球ＫＤ旋转蒸发浓缩仪 (上海玻璃仪器公司 ) ,色谱柱为ＨＰ 5( 30ｍ× 0 .2 5ｍｍ×0 .2 5μｍ)弹性石英毛细管柱 (美国惠普公司 )…     

玻璃毛细管气相色谱讲座 第二讲 玻璃毛细管柱的制备

毛细管色谱柱经过二十多年的不断改进和发展,使它的柱效、柱寿命、重复性、惰性和热稳定性等都得到很大的提高和改善。毛细管柱的制备方法很多,本讲主要介绍载体涂层开管柱(SCOT 柱)的制备。2-1.玻璃和石英毛细管柱的拉制由于玻璃的表面化学惰性比金属好,来源方便,价格便宜、透明性好,所以被作为毛细管柱的材质而广为     

分子筛改性气—液毛细管柱及其性能考察

以原位合成法制备的分子筛膜对玻璃毛细管内壁进行改性后，成功地制备了常规口径及大口径分配ＳＣＯＴ柱，并对毛细管柱的性能进行了评价。     

Cu-M/ZSM-S(M=Ce,La,Ag)催化剂的表征及其对NO直接分解催化活性的研究

考察了用分散法制备的Ｃｕ－Ｍ／ＺＳＭ－５（Ｍ＝Ｃｅ,Ｌａ,Ａｇ）催化剂对ＮＯ直接分解的催化活性,并且用ＸＲＤ、ＳＥＭ、ＴＰＲ、ＸＰＳ及ＩＣＡＰ等手段对催化剂进行了表征。结果表明添加Ｃｅ有利于增加催化剂的铜离子交换度,添加Ａｇ有可能使ＺＳＭ－５分子筛的骨架结构发生改变,从而对催化剂活性产生影响。     

Cu—M／ZSM—S（M=Ce,La,Ag）催化剂的表征及其对NO直接分解催化活性？…

考察了用分散法制备的Ｃｕ－Ｍ／ＺＳＭ－５（Ｍ＝Ｃｅ,Ｌａ,Ａｇ）催化剂对ＮＯ直接分解的催化活性,并且用ＸＲＤ、ＳＥＭ、ＴＰＲ、ＸＰＳ及ＩＣＡＰ等手段对催化剂进行了表征。结果表明添加Ｃｅ有利于增加催化剂的铜离子交换度,添加Ａｇ有可能使ＺＳＭ－５分子筛的骨架结构发生改变,从而对催化剂活性产生影响。     

猪油挥发油成分的气相色谱/质谱法分析

1　引　　言油脂是人类的主要食品之一 ,其主要成分是脂肪酸甘油三酯 ,它参与人体正常生理代谢。油脂香气成分是其微量成分 ,含量一般在油脂总量的 1%以下 ,却构成其各自特征香气。奶油、玉米油、牛油等均有较详细的报道。本文以ＧＣ ＭＳ分析猪油香气成分 ,70种成分被确定。2　实验部分2 .1　主要仪器　ＨＰ5 973气质联用仪 (ＧＣ ＭＳ) ,ＨＰＩＮＮＯＷＡＸ 30ｍ× 0 .2 5ｍｍ× 0 .2 5 μｍ毛细管柱 ,ＮＩＳＴ98谱库。2 .2　ＧＣ ＭＳ条件　进样口温度 2 5 0℃ ,检测器温度 2 80℃ ,柱温 6 0℃ (2ｍｉｎ) 2℃ ｍｉｎ12 0℃ (1ｍｉｎ) 10…     

Blue Rayon人造纤维对多环芳烃的富集作用

1　前　　言ＢｌｕｅＲａｙｏｎ是一种被酞青蓝所染色的人造纤维 ,被许多科学工作者用作多种媒体中微量物质富集的手段。本文主要考察ＢｌｕｅＲａｙｏｎ在大量有机烃类杂质存在的情况下对芘、苯并 (ａ)芘等多环芳烃的富集作用。2　实验部分2 1　气相色谱操作条件　色谱仪 :ＨＰ 5 890Ａ色谱仪 ;ＦＩＤ检测器 ;ＨＰ 5 890Ａ色谱仪 ;ＨＰ 5 971Ａ质谱检测器。色谱柱 :固定相 :ＰＴＥ 5 ,长度 :3 0ｍ ,液膜厚度 :0 .2 5 μｍ ,熔融硅毛细管柱 (Ｓｕｐｅｌｃｏ,Ｉｎｃ.)。柱温 :初始温度 :4 0℃ ;保持时间 :4ｍｉｎ ;升温速率 :8℃ ｍｉｎ;终…     

大孔径毛细柱的研制及评价

大孔径毛细柱在国外(如SUPELCO公司)已有商品出售。国内也有文献报道。我们根据大庆石油管理局需求。研究了不同口径毛细柱的制备方法并对其性能做了考察。 一、大孔毛细柱的制备 (一) 用95硬质玻璃拉制成0.42、0.55、0.7mm不同口径的玻璃毛细管柱。经1∶1盐酸处理后,使用国产甲基乙烯基硅橡胶固定液(相当于OV-1)涂渍。对于口径0.42mm和0.55mm的毛细管柱可采用动态涂渍或静态涂渍,而对于0.7mm口径的毛细管柱,     

食品包装材料中双酚A的极谱测定

1　引　　言双酚Ａ(ｂｉｓｐｈｅｎｏｌＡ ,ＢＰＡ)是近几年新发现的一种“破坏内分泌化学物质 (ｅｎｄｏｃｒｉｎｅｄｉｓｒｕｐｔｉｎｇｃｈｅｍｉｃａｌｓ,ＥＤＣ) ,”已引起各国的广泛关注。其测定方法有ＨＰＬＣ法、ＧＣ ＭＳ法、ＬＣ ＭＳ法、荧光光度法及ＥＬＩＳＡ法等 ,而极谱法未见报道。本研究发现在 0 .7ｍｏｌ ＬＮａＮＯ2 介质中 ,ＢＰＡ的亚硝化产物在电位 (Ｅｐ) -0 .4 1Ｖ(ｖｓ.ＳＣＥ)处产生一个十分灵敏的二阶导数还原波。据此建立了用单扫示波极谱法测定ＢＰＡ的简便方法。2　实验部分2 .1　仪器与试剂　ＭＰ 2型溶出分…     

有机硅结构导向剂法合成ZSM-5分子筛

新型分子筛的合成一直是分子筛研究的热点．引入有机试剂,特别是引入季铵碱,可合成许多新型分子筛［１－４］． Ｄａｖｉｓ等［５,６］报道了利用有机硅 ＴＢＡＳｉ（Ｎ－Ｔｒｉｍｅｔｈｏｘｙｓｉｌｙｌｐｒｏｐｙｌ－Ｎ,Ｎ,Ｎ－ｔｒｉ－ｎ－ｂｕｔｙｌａｍ－ｍｏｎｉｕｍ ｂｒｏｍｉｄｅ）, ＴＰＡＳｉ（Ｎ－Ｔｒｉｍｅｔｈｏｘｙｓｉｌｙｌｐｒｏｐｙｌ－Ｎ,Ｎ,Ｎ－ｔｒｉ－ｎ－ｐｒｏｐｙｌａｍｍｏｎｉｕｍ ｂｒｏｍｉｄｅ）为结构导向剂合成了 ＺＳＭ－５和 ＺＳＭ－１１．通过２９Ｓｉ ＮＭＲ研究证明有机硅进入了分子筛骨架…     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。