共振散射光谱法研究人血清白蛋白与二甲酚橙的反应

对二甲酚橙作为光散射探针测定蛋白质进行了研究,基于人血清白蛋白对二甲酚橙的共振光散射强度的增强效应,建立了测定蛋白质的共振散射光谱法。在pH 4.00的NaOAc-HOAc缓冲溶液中,二甲酚橙只有微弱的光散射强度,但它与蛋白质的缔合物却有较强的共振光散射信号,在λ=517 nm处,光散射强度达到最大,并且与蛋白质浓度在为0.0~10.0 mg.L-1范围呈线性,检出限为0.044 mg.L-1。运用摩尔比法测定二甲酚橙和蛋白质的结合数为132,用于实际样品的分析,测定值与考马斯亮蓝法的结果一致,分析结果的RSD值(n=5)均小于5%。     

酸性铬兰K-OP-牛血清白蛋白体系的共振瑞利散射及共振非线性散射光谱研究及应用

在pH 3.2的邻苯二甲酸氢钾-HCl缓冲液中,酸性铬兰K(ACBK)-OP与牛血清白蛋白(BSA)形成三元离子缔合物,导致共振瑞利散射(RRS)、二级散射(SOS)和倍频散射(FDS)的显著增强,光谱最大散射波长分别位于420,678和340nm。体系的光散射强度与BSA浓度在一定范围内呈线性增强,RRS在0~3.5 mg/L,SOS在0~3 mg/L,FDS在0~3 mg/L范围内对BSA的检出限分别为0.3,0.7和0.8μg/L,据此建立了测定BSA的共振线性(RRS)和共振非线性光散射(RNLS)分析法。以RRS法考察了酸性铬兰K-OP与白蛋白形成三元缔合物的适宜条件、影响因素等。方法可用于合成样品及血清样品中蛋白含量的测定。     

溴代十六烷基吡啶增敏共振光散射法测定乌拉地尔

以稀盐酸介质,固绿FCF作探针,表面活性剂溴代十六烷基吡啶作增敏剂,建立了测定乌拉地尔的共振光散射新方法。在稀盐酸存在下,乌拉地尔与固绿FCF-溴代十六烷基吡啶反应生成离子缔合物,使体系的共振光散射信号明显增强并产生新的共振光散射光谱,最大共振光散射(RLS)峰位于344 nm,乌拉地尔的质量浓度在0. 003～0. 28mg·L-1范围内与体系的共振光散射增强强度(ΔIRLS)呈线性关系,检出限为0. 0028 mg·L-1,加标回收率为98. 96%～101. 3%,相对标准偏差(RSD)(n=5)为2. 1%～2. 6%。该法灵敏、快速,用于市售乌拉地尔药物中乌拉地尔的测定,结果满意。     

共振散射光谱法测定环境水样中痕量锡（Ⅱ）

在pH 4.3的缓冲介质中,痕量锡(Ⅱ)对氯酚红-人血白蛋白-十二烷基硫酸钠体系的共振散射光谱有明显的减弱作用,共振散射强度的减弱程度(△I)与锡(Ⅱ)的质量浓度之间在0.2～4.0μg·L-1范围内呈线性关系,检出限(3S/N)为0.12μg·L-1,用于3件环境水样中痕量锡(Ⅱ)的测定,测定结果的相对标准偏差(n=6)小于3.5 %,加标回收率为95.5%～100.6%.     

钙试剂-蛋白质体系的共振光散射光谱研究

基于蛋白质对钙试剂共振光散射的增强作用,拟定了一种测定蛋白质的共振光散射法。在pH 4.00的水溶液中,钙试剂在595 nm处的共振光散射增强与蛋白质浓度呈线性关系。此方法对人血清白蛋白、牛血清白蛋白的检出限分别可达0.068和0.085μg/mL。同时得到钙试剂与人血清白蛋白和牛血清白蛋白的结合常数(K)以及结合位点数(n)分别为8.15×104mol/L,0.18和7.67×104mol/L,1.5。     

吖啶橙共振光散射法测定酵母核糖核酸

在pH 11.2的B-R缓冲溶液中,吖啶橙与酵母核糖核酸形成缔合物,使酵母核糖核酸的共振散射增强。体系的最大散射波长为333nm,酵母核糖核酸的质量浓度在0.05~15.0mg·L-1范围内与共振散射增强强度(ΔI)呈线性关系,检出限(3s/k)为0.017mg·L-1。据此,提出了一种简单而快速测定酵母核糖核酸的方法。应用此方法测定2个空白合成样品中酵母核糖核酸的含量,测得平均回收率为99.0%,平均相对标准偏差(n=5)为1.3%。     

二苯胺磺酸钠共振光散射法测定牛尿中白蛋白的研究

研究了以二苯胺磺酸钠为共振光散射探针测定牛尿中牛血清白蛋白的分析方法.该方法基于在pH=3.0的Britton-Robinson缓冲溶液中,牛血清白蛋白(BSA)与二苯胺磺酸钠结合后有强烈的共振光散射作用,在λ=469 nm处,共振光散射强度最大且光散射的强度与BSA的浓度成正比.方法简便、快速、灵敏度高,对BSA的检出限为0.18 mg/L,线性范围为0.20～16 mg/L,相关系数r=0.996.该法用于牛尿样品的分析测定,结果满意.     

同步荧光光谱法测定蛋白质

在模拟生理条件下,由于核苷类药物中间体氰基乙基尿嘧啶(CEU)与血清白蛋白相互作用,血清白蛋白的内源荧光发生特异性变化,且体系的同步荧光强度和溶液中血清白蛋白的浓度呈线性关系,据此提出以氰基乙基尿嘧啶为探针,用固定波长同步荧光光谱法测定人血清白蛋白(HSA)和牛血清白蛋白(BSA)的方法.在最佳试验条件下,体系的荧光强度与HSA和BSA的质量浓度分别在1.38～496.2 mg·L-1和1.56～624.0 mg·L-1范围内呈线性关系,检出限(3S/N)分别为0.045 mg·L-1和0.051 mg·L-1.方法应用于人血清及牛血清中HSA及BSA的测定,并以此样品为基体分别加入HSA及BSA标准溶液作回收试验,测得回收率在95.1%～102.5%之间,相对标准偏差(n=6)在0.43%～2.72%之间.     

海藻酸钠-[C_(16)mim]Br体系共振光散射法测定离子液体[C_(16)mim]Br

在pH 5.0的B-R缓冲介质中,海藻酸钠能与[C16mim]Br离子液体形成离子缔合体系,使[C16mim]Br的共振散射增强。体系在最大散射波长392 nm处,[C16mim]Br的质量浓度在1.9~12.0 mg.L-1范围内与共振散射增强强度(ΔI)呈线性关系,检出限(3s/k)为76.7μg.L-1。据此提出了一种简单而快速测定[C16mim]Br的方法,应用于测定水样中[C16mim]Br,测得回收率在97.8%~102.3%之间,相对标准偏差(n=6)在1.87%~3.01%之间。     

全氟辛烷磺酸与蛋白质体系的共振光散射光谱及其分析应用

研究了牛血清白蛋白(BSA)与全氟辛烷磺酸(PFOS)相互作用的共振光散射(RLS)光谱,建立了PFOS的共振光散射分析方法。 在pH值为4.1的BR缓冲溶液中,全氟辛烷磺酸根阴离子与质子化的BSA通过静电引力和疏水作用形成离子缔合物,引起共振光散射强度(IRLS)显著增强,最大散射波长位于285.0 nm处,增强的散射信号强度与PFOS浓度在0.2～25.0 μmol/L范围内呈线性关系,据此建立了测定PFOS的光散射分析方法,检出限为20.0 nmol/L。 讨论了体系的最佳反应条件及外来物质的干扰,并探讨了反应机理。 建立的共振光散射法用于环境水样中PFOS的测定,RSD≤4.4%。     

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。