蛋白质-SDS-罗丹明B体系的共振光散射光谱及其分析应用

研究了阴离子表面活性剂十二烷基硫酸钠(SDS),阳离子染料罗丹明B,与蛋白质相互作用的共振光散射(RLS)光谱及用于蛋白质的测定.实验表明,在pH 4.35的酸性介质中,SDS的共振光散射强度较小,它与蛋白质结合后,共振光散射强度能得到增强,但加入阳离子染料罗丹明B后,共振光散射强度显著增强.在λ=332.0 nm处,ΔIRLS最大,并且增强的共振光散射信号与蛋白质的浓度成正比.据此建立了一种测定蛋白质的新方法,该方法灵敏度高,对HSA的检出限达到1.9 ng/mL,线性范围为0.01～5.0 μg/mL.用于人血清样品中蛋白质的测定,回收率为94.0%～105.5%.     

表面活性剂和染料探针共振光散射法测定蛋白质

在pH为2.1的Britton-Robinson缓冲溶液中,蛋白质与十二烷基磺酸钠和吖啶红作用形成聚集体,导致体系产生较大的共振散射光(RLS)强度,并且RLS的增强程度与蛋白质的浓度呈线性关系,据此建立了测定蛋白质含量的方法.人血清白蛋白(HSA)和牛血清白蛋白(BSA)分别在0.03～3.0μg/mL和0.2～7.0μg/mL的浓度范围内与增强的共振光散射强度有良好的线性关系,相应的检测限分别为0.0119μg/mL和0.026μg/mL.对体系的反应机理进行了讨论.将方法用于人血清中蛋白质含量的测定,并将分析结果与考马斯亮蓝法进行了对照.t-检验证明,两种方法无显著性差异.     

花菁-脱氧核糖核酸的共振光散射光谱及其分析应用

研究了一种苯并噻唑阳离子花菁与脱氧核糖核酸(DNA)作用的共振光散射光谱,在pH 6.0的六次甲基四胺-HCl缓冲介质中,痕量DNA的加入使花菁在590nm的共振光散射强度显著增强。在最佳实验条件下,增强的共振光散射强度与DNA浓度具有良好的线性关系,据此建立了一种测定DNA的共振光散射光谱法。方法的线性范围为:小牛胸腺DNA(CT DNA),0～20μg/mL,鱼精子DNA(FS DNA),0～15μg/mL;检出限分别为0.005μg/mL和0.008μg/mL。该方法已用于合成样品中DNA的测定。     

虎红-牛血清白蛋白共振光散射光谱研究及其分析应用

基于在pH3.0的BR缓冲溶液中蛋白质的加入使虎红的共振光散射信号增强,建立了一种蛋白质测定的新方法.详细地探讨了pH、染料用量、表面活性剂、离子强度、共存物质等对信号的影响.牛血清白蛋白浓度在0～4.0μg/mL范围内与体系散射强度呈线性关系,检出限为0.01718μg/mL.该方法用于合成样品中牛血清白蛋白的测定,...     

共振光散射光谱研究噻嗪红R与牛血清白蛋白的作用及其分析应用

研究了噻嗪红R(Thiazine red R,TR)与牛血清蛋白(BSA)作用的共振光散射(RLS)光谱特征。考察了各种影响因素,并计算出了BSA与TR的结合比(质量之比)为1.25。结果表明,在优化条件下体系的RLS强度与蛋白质浓度在一定范围内具有良好的线性关系,据此建立了一种蛋白质测定的新方法。在最佳实验条件(TR,2.0×10-5mol/L;pH2.36)下,BSA的线性范围是0.01~5.0μg/mL,检出限为1.4ng/mL。该方法已用于合成样品及尿液的测定。     

同多酸和染料探针共振光散射法测定蛋白质

在酸性条件下,铬黑T、钼酸铵与蛋白质形成聚合物,使体系的共振光散射明显增强。据此建立了利用共振光散射技术测定总蛋白含量的新方法。在最佳条件下,体系的最大散射峰位于555nm处。共振光散射增强的程度与蛋白质的浓度呈良好的线性关系。牛血清白蛋白和人血清白蛋白的线性范围分别为0.20～10.0μg/mL和0.10～8.0μg/mL,检出限为0.050μg/mL和0.039μg/mL。方法已用于人血清样品的分析,并与考马斯亮蓝的测定结果进行了比较,两者无显著性差异。     

血清白蛋白的铅(Ⅱ)-抗坏血酸络合吸附波法测定

在pH9．2的H3BO3-NaOH缓冲溶液中,血清白蛋白使铅(Ⅱ)-抗坏血酸络合物在-0．51V(vs．SCE)处的络合吸附波电流降低,电流降低值与加入的牛血清白蛋白(BSA)或人血清白蛋白(HSA)的浓度在一定范围内呈线性关系。BSA在2～38μg／mL范围内,HSA在2～35μg／mL范围内呈线性关系,检出限均为1μg／mL。应用该法测定了人血清样品中蛋白质的含量,结果令人满意。     

光谱法研究二甲酚橙-Cu(Ⅱ)配合物与蛋白质的相互作用

研究了二甲酚橙(XO)-Cu(Ⅱ)配合物与牛血清蛋白(BsA)相互作用的共振散射光谱(RLS)和电子吸收光谱,建立了一种利用金属配合物为探针测定痕量蛋白质的分析方法.在pH 2.50的Britton-Robinson缓冲溶液中,XO-Cu(Ⅱ)与BSA作用后在λ=557 nm处出现一增强的共振散射峰,且增强的RLS强度与蛋白质的浓度呈线性关系.在选定的优化条件下,线性范围为0.18～15μg/mL.线性方程为I(Rts)=46.5+64.8ρ(μg/mL),r=0.998,方法检出限为0.15μg/mL.该方法用于牛尿及牛血样品分析测定.对二甲酚橙-Cu(Ⅱ)配合物与蛋白质的相互作用的研究表明,二甲酚橙-Cu(Ⅱ)配合物与蛋白质之间主要存在的相互作用是静电引力.     

樱桃红共振光散射光谱法测定牛血清白蛋白

研究了以樱桃红为共振光散射探针测定牛血清白蛋白的分析方法。在pH 3.58的BR缓冲溶液中,樱桃红与牛血清白蛋白(BSA)相互作用形成复合物,导致共振光散射(RLS)光谱明显增强,最大RLS峰位于340 nm处。由此建立检测痕量BSA的新方法。在优化实验条件下,RLS强度与BSA浓度的线性范围为1.0～60.0μg/mL,检出限为0.15μg/mL。方法可用于牛尿样品的分析。     

丽春红G 用于人血清样品中总蛋白的共振光散射测定

在酸性介质中 ,丽春红G (PonceauG ,PG)与牛血清白蛋白 (BSA)、人血清白蛋白 (HSA)、溶菌酶 (Lys)及γ 球蛋白 (γ IgG)等蛋白质作用产生共振光散射 (RLS)增强信号 ,最大散射峰位于 2 88nm处。在最佳酸度和离子强度下 ,增强RLS强度在 2 88nm处与蛋白质的浓度呈线性关系 ,用于测定BSA、HSA、Lys、γ IgG的检出限均在 2 5 μg L以下。本方法成功地应用于合成样和人血清样品的测定 ,测量结果与考马斯亮蓝法一致     

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.     

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。     

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.

     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

解决能源问题的新途径——光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。