均匀设计在蚕蛹虫草和冬虫夏草活性成分分析中的应用

采用均匀实验设计方法快速找到蚕蛹虫草活性成分的高效液相色谱最优分离条件;将该优化条件用于蚕蛹虫草和冬虫夏草的水溶性成分的分离取得满意结果,并对部分组分进行了定性定量分析;均匀实验设计方法可较快找到复杂未知或半未知体系的色谱分离条件。     

高效离子交换色谱法分离皖南尖吻蝮蛇毒活性组分

采用高效离子交换色谱法对经初步分离的皖南尖吻蝮蛇毒活性成分进行进一步的分离纯化。采用线性梯度洗脱,得到蝮蛇毒活性组分纯品,并用峰面积归一化法计算其含量为４５．４１％左右,纯度在９０％以上。     

SE-HPLC-ICP-MS联用技术在富硒蛹虫草硒蛋白形态分析中的应用研究

从富硒培养的虫草中提取可溶性蛋白质, 经过(NH4)2SO4分级盐析, 采用ICP-MS对不同盐析组分中蛋白及硒分布进行测定, 结果表明, 富硒蛹虫草的可溶性硒含量占总硒含量的69.3%以上, 在所得的各级蛋白组分中, 除A组分(0~30%饱和度的盐析)外, 其它各组分均存在含硒蛋白, 其硒含量高低顺序为B组分(30%~50%饱和度的盐析)>C组分(50%~75%饱和度的盐析)>D组分(75%~100%饱和度的盐析)>A组分. 采用SE-HPLC-ICP-MS联机技术对样品中的硒蛋白进行分离检测, 结果表明, 其分子量分布在114000和1000之间, 且含量各异. 进一步研究结果表明, 硒在虫草体内参与了蛋白的合成, 这对于以蛹虫草为载体将无机硒有机化具有重要意义.     

蛹虫草中硒的赋存形态及蛋白硒分析

为研究蛹虫草中硒的赋存形态,并进一步探究蛹虫草硒蛋白组分中硒含量的分布,以蛹虫草子实体为研究对象,用DAN荧光法测定了硒含量,用连续提取法进行了蛋白硒分析。结果表明,蛹虫草最高硒含量为89.486mg·kg-1,有机硒占85.96%;蛹虫草中蛋白硒、多糖硒和核酸硒分别占有机硒的71.4%~77.1%、19.7%~32.3%和0.138%~2.727%;在硒蛋白组分中虫草盐溶性蛋白、水溶性蛋白、醇溶性蛋白和碱溶性蛋白结合硒分别占总蛋白硒的55.13%~56.80%、20.47%~24.60%、15.30%~16.49%和2.99%~3.35%。蛹虫草具有很强的富硒能力;在蛹虫草子实体中,有机硒主要与蛋白质、多糖、核酸等生物大分子结合,其中蛋白质结合硒是硒的主要赋存形态;在蛋白质组分中,又以盐溶性蛋白质结合硒量最多。     

高效液相色谱分离纯化血管紧张素转换酶活性抑制肽

采用分步高效液相色谱法首次从菠菜核酮糖双磷酸羧化酶(英文缩写为Rubisco)的胃蛋白酶-胰酶复合酶水解产物中分离纯化了血管紧张素转换酶(ACE)活性抑制肽。水解产物经ODS柱分离得到活性组分,这些活性组分再依次经过氨基柱(PhA) 氰基柱(CN)和硝基苯乙基柱(NPE)4种色谱柱分离后,得到4种高度纯化的具有抑制ACE活性的多肽。经蛋白质序列自动分析仪测定,4种多肽的结构分别为MRWRD,MRW,IAYKPAG和LRIPVA。采用固相多肽合成法分别合成了这4种肽,并采用测定ACE活性抑制率的方法评价其     

十二烷基糖苷的反相高效液相色谱分析

烷基多苷（APG）是一类环保型非离子表面活性剂,由脂肪醇与糖制备,为单糖苷和多糖苷的混合物.受分离方法的限制,难以得到其中各组分的纯品,因此APG的组成测定一直未得到很好的解决.本文采用制备色谱对其进行分离,经核磁共振氢谱（^1H NMR）确定各组分的结构,用高效液相色谱（HPLC）分析测定了相对质量校正因子（f）,为完善APG的结构分析及质量控制奠定了基础.     

气相色谱法分析气雾型杀虫剂产品中的硫酰氟和环氧乙烷

建立了用气相色谱校正归一法分析气雾杀虫制剂产品中硫酰氟、环氧乙烷的方法。色谱条件：色谱柱为Porapak QS（2.0 m×3 mm）,检测器为热导检测器。在Porapak QS色谱柱上硫酰氟、环氧乙烷能与其他组分很好地分离,分离度大于2.0。硫酰氟含量（质量分数）为0.341%~54.6%、环氧乙烷含量为0.341%~34.1%时,目标化合物的含量与其峰面积呈现良好的线性关系;硫酰氟检测限为0.0103%,环氧乙烷检测限为0.0614%。精密度实验结果表明,在线性范围内,峰面积的相对标准偏差（RSD）小于3.0%。该法操作简便、快速,准确性高,重复性好,对同一样品的6次平行测定的RSD小于2%,可作为该类产品的质量控制方法。     

La(NO3)3对蛹虫草活性物质含量的影响EI北大核心CSCD

蛹虫草是一种著名的药用和食用真菌,研究者们常在培养基中添加亚硒酸钠、Fe SO4等无机物来提高蛹虫草活性物质的含量。本文采用高效液相色谱法和紫外分光光度法测定了La(NO3)3处理后蛹虫草活性物质的含量,探究La(NO3)3对蛹虫草活性物质含量的影响。结果表明,在实验浓度范围内,10,50和200 mg·L-1这3个浓度对蛹虫草的活性物质含量影响较大。La(NO3)3浓度为10 mg·L-1时,对喷司他丁、虫草酸和多糖合成具有促进作用,其含量分别为空白组的6.2倍、2.4倍和1.3倍,La(NO3)3对蛹虫草的腺苷和N6-2-羟乙基腺苷合成具有抑制作用,其含量仅为空白组的24.29%和16.87%。La(NO3)3浓度为50 mg·L-1时,对虫草素合成具有显著促进作用,其含量为空白组的8.2倍,La(NO3)3对多糖合成具有抑制作用,其含量仅为空白组的73.14%。La(NO3)3浓度为200 mg·L-1时,对腺苷和N6-2-羟乙基腺苷合成具有促进作用,其含量分别为空白组的1.5倍和2.6倍。La(NO3)3对麦角甾醇和蛋白质的含量未产生显著影响(P>0.05)。     

反相高效液相色谱法同时检测发酵液中的L-苯丙氨酸和β-苯乙醇

β-苯乙醇是香料和化妆品行业中使用量最多的香味成分。利用酵母的Ehrlich代谢途径,把L-苯丙氨酸生物转化为β-苯乙醇是一种很好的生产天然β-苯乙醇的方法。在β-苯乙醇产生菌的菌种选育和发酵工艺研究过程中,需要建立一种对生物转化体系中L-苯丙氨酸和β-苯乙醇组分和含量的快速检测方法。本文利用反相高效液相色谱法同时测定发酵液中的L-苯丙氨酸和β-苯乙醇。该法无需衍生和梯度洗脱,有较宽的线性范围及较低的检测限,可作为微生物转化发酵体系中L-苯丙氨酸和β-苯乙醇的定量测定方法。     

快速高效液相色谱法测定卷烟主流烟气中的酚

简单酚类化合物是卷烟主流烟气中的一类重要有害成分,采用液相色谱分离检测酚类化合物已有许多文献报道。为了进一步缩短分离时间,我们采用快速高效液相色谱法（HPLC）测定了卷烟主流烟气中的酚,主要酚在2．0min内可达到基线分离,取得令人满意的结果。     

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。