徐州地区胆结石的溶剂萃取的FTIR研究

胆石病是徐州地区的多发病之一,针对徐州地区临床术中取出的五类胆结石利用系列溶剂萃取,用傅里叶变换红外光谱(FTIR)分别表征萃取前后的成分、结构及形态变化。结果表明:所取的五类徐州地区胆结石分别为胆固醇型、难溶物分别为胆红素盐、蛋白质的胆固醇为主的混合型、棕色色素型和黑色色素型胆结石。蛋白质为胆结石的形成提供沉淀基质,对于胆结石成核具有重要意义;胆结石难溶物中胆固醇和羟基碳酸磷灰石相伴而生,羟基磷灰石与胆固醇存在相互作用,促使其结晶析出,从而加速胆结石的形成。结果可以为胆结石的临床诊断、治疗及预防提供一定的参考。     

胆结石中蛋白质的傅里叶变换红外光谱和表面增强拉曼光谱研究

用氯仿、乙醚、乙醇和盐酸等溶剂溶解一组人体胆结石，获取难溶物；用傅里叶变换红外光谱和表面增强拉曼光谱对难溶剩余物进行研究。结果显示，结石难溶物主要由胆红素盐和蛋白质组成，结石中的蛋白质的二级结构以α螺旋和无规卷曲构象为主，其中α螺旋构象成分较多。讨论了蛋白质在胆结石形成中的作用。     

火焰原子吸收光谱法间接测定烟草中的烟碱含量

基于盐酸介质中雷氏氨盐的室温下与烟碱定量形成难溶配合物的性质，采用火焰原子吸收光谱法测定反应体系中变化的铬量，根据反应计算出样品中烟碱的含量。方法用于测定烟草中的烟碱含量，回收率91.6%－105.5%，相对标准偏差1.4%-5.2%，结果满意。     

应用ICP-AES技术测定胆管胆色素结石粉及其难溶部分中的元素组分

用ICP-AES技术研究了胆石粉的处理过程,选择了合适的实验条件,并做了精密及回收率实验。为21例结石粉及其难溶部分进行了元素测定。计算了残留元素百分比,为医学研究提供了有用数据。     

Infrared Absorption Intensity Analysis as a New Tool for Investigation of Salt Effect on Proteins

通过观测红外光谱的强度变化研究了在不同温度下盐离子对谷氨酸和三种水溶性蛋白质(细胞色素C、DsbC和DsbC-G49R)的影响. 证实了Onsager反应场理论. 区分并且定义了随温度变化的蛋白质盐效应盐溶过程和解离过程. 同时利用Van't Hoff关系式对实验结果进行线性拟合,获得了蛋白质及其二级结构在上述两个过程中的热力学常数.     

植物色素的光声光谱研究

测定了纸色谱分离的极为微量的六种植物色素的光声光谱，并与相应色谱斑点溶出物的吸收光谱进行对照，表明光声光谱对植物色素的鉴定简便有效，海藻类别众多，所含色素体系各有特征，本文报道了绿色藻，红藻和褐藻的光声光谱，并用导数光谱法明确了这些藻类的色素分布特征。     

莲子蛋白组分二级结构的研究

对莲子蛋白质进行了Osborne蛋白质分类。采用傅里叶变换红外光谱(FTIR)对清蛋白、球蛋白、醇溶蛋白和谷蛋白进行二级结构分析。应用去卷积和曲线拟合方法对四种蛋白组分的酰胺Ⅰ和Ⅲ带进行分析,清蛋白和球蛋白之间以及醇溶蛋白和谷蛋白之间各相应子峰峰位和二级结构峰面积百分比差异较小,但前两者各相应子峰峰位与后两者略有差异;而前两者各相应二级结构峰面积百分比与后两者有较大差异,特别是前两者的各相应有序结构(α-螺旋+β-折叠)峰面积的百分比明显大于后两者。用0.1 mol.L-1NaCl溶液提取的球蛋白和清蛋白有序结构含量均在55%左右,而醇或碱提的醇溶蛋白和谷蛋白的有序结构含量仅为40%左右,盐提的蛋白质二级结构有序性和稳定性更高。     

珍珠层独特的反射光谱特征及其成因

采用反射光谱、扫描电镜及理论模拟计算对大珠母贝珍珠层的结构色及微结构进行了系统的研究。结果表明:(1)大珠母贝珍珠层文石板片厚度从生长端到壳中区显著减小, 从540减至340 nm, 导致同级别反射峰波长呈现明显的蓝移现象;(2)大珠母贝珍珠层的结构色是由文石板片和蛋白质层构成的多层薄膜结构和黄色素的共同作用决定的。     

用19F NMR参比积分法测Ba2+与18-冠-6络合物的稳定常数

提出了一种间接的但十分简单的方法测定Ba²⁺与18-冠-6的络合平衡常数。在不同浓度的18-冠-6水溶液中,分别加入难溶盐BaF₂。使其饱和,然后对各溶液进行¹⁹F NMR定量测定。根据络合平衡和难溶盐的溶解平衡,确定了Ba²⁺与18-冠-6的络合平衡常数。     

胆石病人胆汁的光谱及稳定性分析

采用红外光谱及二阶导数谱、紫外光谱、动态激光光散射粒度分析、Zeta电位等测试与分析方法,对胆石病人的原胆汁及经离心处理后的胆汁进行了分析。结果表明,胆石病人的胆汁是一个非均匀体系, 处于相对不稳定状态;离心后的胆汁聚沉物主要含有胆固醇、胆红素及其钙盐、蛋白、磷脂等物质,与该病人胆石核心的主要成分非常相似。胆汁中磷脂类囊泡的破坏以及一些难溶性钙盐的生成是影响胆汁稳定性及胆石形成的主要因素。磷脂和蛋白等有机基质在该病人结石的成核过程中可能起诱导和调控作用。     

Investigation of Surface-Enhanced Raman Spectra of Human Gallstones on Colloidal Silver

The surface-enhanced Raman scatterihg (SERS) spectra of human gallstones is investigated. Complicated Raman bands were due to multiple components that include bilirubin, bilirubinate salts, cholesterol, fatty salts and proteins. The results suggest that besides bilirubin and cholesterol, fatty salts and proteins may play an important role in the formation of gallstone. The experimental data supply an useful information for the research of the formation mechanism of gallstones.     

Investigation of Surface-Enhanced Raman Spectra of Human Gallstones on Colloidal Silver

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胆结石的FT－Raman光谱研究

胆结石的ＦＴ－Ｒａｍａｎ光谱研究徐智勇，李维红，王立波，许振华，吴瑾光（北京大学化学与分子工程学院，稀土材料化学与应用国家重点实验室北京１００８７１）ＴｈｅＩｄｅｎｔｉｆｉｃａｔｉｏｎｏｆＴｈｒｅｅＤｉｆｆｅｒｅｎｔＴｙｐｅｓｏｆＧａｌｌｓｔｏｎｅｓ...     

Identification of cholesterol gallstones using in vitro low-fluence laser-induced fluorescence spectroscopic analysis

Identifying the chemical composition of gallstones may be important in certain cases of calculus biliary disease when planning a dissolution therapy or a fragmentation of the calculi using pulsed lasers. The present study was conducted in vitro to evaluate the feasibility of distinguishing cholesterol gallstones from pigment stones. We propose an identification method in which the stone fluorescence spectrum, induced by a low fluence laser, is recorded using an optical multichannel analyser. Fluorescence spectra of twenty-two stones were recorded together with the fluorescence spectra of various pure compounds likely to compose the gallstones, using successively four different pump lasers (_p=308 nm, 337 nm, 423 nm, 469 nm). The fluorescence spectra of cholesterol gallstones are quite different from the pigment ones. Ratios of fluorescence intensities taken at three different wavelengths enable one to distinguish easily between cholesterol and pigment stones.     

Complementary use of the Raman and XRF techniques for non-destructive analysis of historical paint layers

The portable XRF spectrometer has been applied in situ for the non-destructive elemental mapping of the pigment components of the XV c. mural painting and frescos of the Little Christopher chamber in the Main Town Hall of Gdańsk, Poland. For a sufficiently large data collection the principal component analysis (PCA) was applied in order to associate the most intense lines of the elements Ca, Cu, Fe, Pb, and Hg in the XRF spectra with the palette of colors: white, brown, green, blue, red, yellow, and black observed in the painting. This allowed to limit the number of extractions of the micro-samples for the complementary Raman measurements thus assuring the practically non-destructive character of the entire analysis. The reliable identification of the pigment compositions was based on coincidence of the XRF, PCA and the Raman results which confirmed the presence of the chalk, malachite, azurite, red lead, mars red, mars yellow and candle black in the historical paints, except of the carbon-based black pigment being out of the XRF detection range. Different hues of the green paint were specified and the variety of the red and brown ones was ascribed to compositions of the Pb- and Fe-based red pigments (Fe₂O₃ and Pb₃O₄) with addition of the vermilion (HgS) and carbon black, in agreement with literature. The traces of elements: Ba and Sr, Sb and Mo, and also Cd, were ascribed to the impurities of Ca, those of some ochre pigments, and to the soluble Cd salts, respectively.     

胆红素络合物的表面增强拉曼光谱研究

本文通过对近红外激发傅里叶变换拉曼光谱(NIR-FT-Raman)与表面增强拉曼散射(Surface Enhanced Raman Scattering,SERS)技术的联用,测得胆红素及其络合物Na     

Reversible solvent swelling in pigment gallstones

The reversibility of solvent swelling and the existence of an equilibrium swelling ratio, q_eq, has been established for pigment gallstone particles. A simple technique was devised to demonstrate that solvent imbibition in pigment gallstone particles is reversible. This finding confirms unequivocally that the molecular makeup of pigment gallstones involves polymer networks. In addition, this new method permits serial direct observation of the interactions between pigment gallstone particles and the solvent. Application of the technique to other network polymers should be readily possible.     

复合氧化物纳米粉体颜料的制备和表征

印染行业重点技术发展的目标之一就是研制开发高效、环保、安全的新型染化料,为了解决纺织印染中的废水污染问题,发展无水印染新技术,是一个引起人们广泛关注的新研究方向。我们受红宝石,蓝宝石结构特征的启发,尝试采用均相沉淀法合成以α-氧化铝为基质,通过少量掺杂呈色离子的复合氧化物颜料。实验中,将结晶氯化铝和一定比例的发色离子氯化物混合,用适量的蒸馏水溶解,再溶入尿素和聚乙烯吡咯烷酮,超声振荡均匀,将上述液体加热回流,煅烧反应后的产物,得到纳米无机颜料。通过XRD测定样品的晶型和纯度,确定新型颜料的主体成分是α-氧化铝,用紫外可见光谱仪测试样品的漫反射光谱,发现掺杂离子周围的配位环境变化导致吸收峰谱带发生变化。在此基础上用分光密度仪表征样品的色度,应用SEM进行微观形貌分析,样品粒径范围在200～300nm。将制成的复合氧化物颜料用饱和盐酸浸泡,对浸出液进行ICP测试,发现掺杂离子溶出量非常少,说明新型颜料具有良好的化学稳定性。上述结果说明,这类新型无机纳米粉体颜料各种耐性良好、无毒害,可以满足熔体纺丝要求,有望在无水印染方面得到应用。     

Thermally stimulated luminescence of urine salts

We investigated thermally stimulated luminescence (TSL) of urine salts in the normal state and with oxalate, urate, and phosphate salts. We found that the presence of pathological salts leads to a decrease of TSL intensity and to the appearance of additional TLS bands with maxima at 118 and 205 K in addition to the characteristic bands at 173 and 260 K. The TLS bands are related to the urine components. The TSL intensities of urine salts of different chemical composition are compared. The thermal activation energy of the strongest TSL bands is determined. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 74, No. 4, pp. 548–551, July–August, 2007.