A modified HPLC method for the determination of aspartic acid racemization in collagen from human dentin and its comparison with GC

The D/L ratio of aspartic acid enantiomers in proteins of low turnover is generally accepted as a reliable procedure for age determination. In our study, twelve samples of eyetooth dentin were analyzed for age determination. The pure insoluble collagen isolated from eyetooth dentin was obtained by an EDTA demineralization process. Free amino acids obtained after collagen hydrolysis were converted into o-phthaldialdehyde-N-acetyl-L-cysteine (OPA-NAC) derivatives for HPLC analysis under modified conditions and into trifluoroacetic acid isopropyl esters for GC analysis, respectively. The modified HPLC procedure used phosphate buffer and acidified sample matrix prior to injection which resulted in suppression of peak tailing of both diastereomers, thus allowing achievement of both good selectivity and good resolution. To ensure the high accuracy of the developed method the other parameters, i.e. specificity, precision, linearity, LOD, and LOQ, were also determined. Nine collagen samples covering the age range of 18 to 84 years were used for the determination of coefficient of racemization (KR) and calculation of parameters for age estimation. The regression equations for the data set analyzed were as follows: KR= 0.0005 x age + 0.0262 (R2 = 0.9639) for HPLC, and KR= 0.0006 x age + 0.0319 (R2 = 0.9374) for GC, respectively.     

高效液相色谱法测定金菊泡腾片中绿原酸的含量

采用Nucleosil C18(250mm×4.6mm,4.5μm)色谱柱,以甲醇-磷酸水溶液(pH=3.0)为流动相,其比例为25∶75,检测波长为327 nm,流速1.0 mL/min,柱温29 ℃,建立金菊泡腾片和双黄连口服液中绿原酸含量的高效液相色谱(HPLC)测定方法.绿原酸浓度在0.02-0.1 mg/mL与峰面积积分值呈良好的线性关系,A=0.9394C 0.3674(r=0.9991).该方法灵敏、简便、重现性好、结果准确,可用于金菊泡腾片中绿原酸含量的测定和产品质量控制.     

谷氨酸钠溶液514nm激光拉曼光谱受环境光影响的研究

探讨了环境光的存在对谷氨酸钠溶液的514 nm绿色激光激发的拉曼光谱的影响.研究表明不同的环境光、自然光和室内荧光灯光均会对514 nm激光拉曼光谱产生干扰,存在着特征干扰峰.自然阳光干扰较小;而荧光灯光表现为1127、2107 cm-1和2170 cm-1等3个明显尖锐的脉冲峰,不能忽略.建议在进行谷氨酸钠溶液514 nm绿色激光拉曼光谱检测时,须在暗室或暗罩中进行,以完全隔离环境光的影响.     

Strength measurements of silica optical fibers under severe environment

Optical fibers are key components in telecommunication technologies. Apart from optical specifications, optical fibers are expected to keep most of their physical properties for 10–20 years in current operating conditions. The reliability and the expected lifetime of optical links are closely related to action of the chemical environment on the silica network. However, the coating also contributes largely to the mechanical properties of the fibers.The aim of this work was to study the strength and the mechanical behavior of the silica optical fibers in an acid environment and with a permanent deformation. A container with ammonium bifluoride acid salt was plunged into hot water at different temperatures (55 and 75 °C). This emitted acid vapors which attacked the optical fibers for a period of 1–18 days. An aging study was performed on silica optical fibers with standard polyacrylate coating and with hermetic carbon coating. A dynamic two-point bending bench at different faceplate velocities (100, 200, 400 and 800 μm/s) was used. For comparison, the same dynamic measurements were also carried out on non-aged fibers.After acid vapor condensation, salt crystal deposits on the fibers were displayed using an electron scanning microscope. These crystals became visible to the naked eye from the seventh day.     

Purification of carbon nanotubes grown by thermal CVD

We show the results of a set of purifications on carbon nanotubes (CNT) by acid and basic treatments. CNTs were obtained by thermal decomposition of camphor at 850 °C in a CVD growth system, by means of a growth process catalyzed by iron clusters originating from the addition of ferrocene in the precursors mixture. The purification procedures involved HNO₃, H₂SO₄, HSO₃Cl and NaOH for different process temperatures.As-grown CNTs showed a consistent presence of metal catalyst (about 6 wt%), evidenced by TGA. The purification treatments led to a certain amount of opening of the CNT tips, with a consequent loss of metal catalyst encapsulated in tips. This is also confirmed by BET analysis, which showed an increase of the surface area density of CNT after the purification.FT-IR and XPS revealed the presence of carboxylic groups on the CNT surface chemically modified by the harsh environment of the purification process.Among the various treatments that have been tested, the 1:3 solution of nitric and sulphuric acid was the most effective in modifying the CNT surface and inducing the formation of functional groups.     

高效液相色谱-光电二极管阵列检测器联用检测不同产地荆芥中乌索酸和齐墩果酸

建立反相高效液相色谱-光电二极管联用法同时测定了荆芥中乌索酸和齐墩果酸的含量。色谱柱为Kromasil C18柱(250mm×4.6mm,5μm),流动相为甲醇-水(86∶14),流速0.8mL.min-1,光电二极管阵列检测器(PAD),检测波长210nm,柱温25℃。在选定色谱条件下线性范围良好,乌索酸和齐墩果酸的样品加样回收率分别为98.6%和99.2%,RSD为1.1%和1.9%。方法简便,分离效果好,可用于荆芥中乌索酸和齐墩果酸含量的测定。     

THE STUDY OF INTERACTION OF SOLID-LIQUID ADSORPTION SYSTEM BY USING THE FLOW INJECTION-SPECTROPHOTOMETRY SYSTEM

1. INTRODUCTION Flow injection analysis is a method that a determinate volume of sample is injected to an airless and continuous flow carrier consisted of suitable liquids, and then is put into a detector to be record absorbency, electrode potential and other physical parameters. This automatic analytical method is characterized by fixed time, quantified sampling, less sampling and good system stability [1]. The new automatic analysis for liquid has been developed quickly since Ruzi…     

Chemistry and key structural features of oxyhydroxy-fluorides: relationships with the acidic character, thermal stability and surface area

The stability of Al, Cr and Fe hydroxy-fluorides MF_3−x(OH)_x which adopt the hexagonal-tungsten-bronze (HTB)-type structure has been discussed by considering the lability of water coordinated to metals from a kinetic point of view. Thus, in the case of Al or Fe compounds, the easy departure of water contributes to the stabilization of fluoride ions as well as isolated hydroxyl groups around the metal, leading to the formation of the HTB structure. The stabilization of the HTB structure with respect to another structural type, the pyrochlore, with a lower density, is governed by this kinetic feature as well as the ability of fluorinated salts used as precursors to attract hydroxyls. Al(III) and Fe(III) represent the strongest acidic cations and the associated HTB-type structure containing isolated OH groups can easily be stabilized. In the case of Cr, a mixture of pyrochlore and HTB-type structure is generally obtained. We have succeeded in preparing, using supercritical medium, new (Fe, Cr) oxyhydroxy-fluorides which exhibit edge-shared octahedra and large 1D tunnels. These compounds can be considered as potential candidates for acid catalysts.     

Periodic Mesoporous Silicas and Organosilicas: An Overview Towards Catalysis

Micelle-templated mesoporous and organic–inorganic hybrid mesoporous materials are important in many fields of material research, especially for hosting catalysts in confined space. Among this class, the recent discovery of periodic mesoporous organosilicas (PMOs) represent an exciting new group of organic–inorganic nanocomposites targeted for a broad range of applications ranging from catalysis to microelectronics. Compared to the earlier generation of organic–inorganic hybrid mesoporous samples, obtained by the cocondensation reaction or by the grafting reaction, PMOs represent the right combination of organic and inorganic groups in the frame wall positions. This article reviews the current state of art in organic–inorganic hybrid mesoporous material research with special emphasis over periodic mesoporous organosilica materials having various redox centers (Ti, V, Cr) suitable for oxidation reactions as well as acidic sites (Al, –SO₃H) for the organic transformation of bulky molecules.     

Acid reflux and hoarseness

The aim of this study was to investigate the prevalence of acid reflux in patients complaining of hoarseness where no organic disease or functional dysphonia could be found. We also aimed to determine whether anti-reflux treatment improved their symptoms. Patients were not selected on the basis of symptoms of reflux. Fifty patients with hoarseness took part in a prospective study that sought to establish objectively whether acid reflux was present. All patients were given a 6-week course of ranitidine and Gaviscon. Patients were asked to score their voice quality before and after treatment. Although 72% of patients complained of heartburn more than once a week, only 40% proved to have acid reflux. Although subjective improvement after anti-reflux treatment was found in a larger proportion of those with than without proven reflux, the conclusions that can be drawn are limited as there were no satisfactory objective measurements of voice or controls.