Application of HPLC to measure vanadium in environmental,biological and clinical matrices

Vanadate and vanadium compounds exist in many environmental, biological and clinical matrices, and despite the need only limited progress has been made on the analysis of vanadium compounds. The vanadium coordination chemistry of different oxidation states is known, and the result of the characterization and speciation analysis depends on the subsequent chemistry and the methods of analysis. Many studies have used a range of methods for the characterization and determination of metal ions in a variety of materials. One successful technique is high performance liquid chromatography (HPLC) that has been used mainly for measuring total vanadium level and metal speciation. Some cases have been reported where complexes of different oxidation states of vanadium have been separated by HPLC. Specifically reversed phase (RP) HPLC has frequently been used for the measurement of vanadium. Other HPLC methods such as normal phase, anion-exchange, cation-exchange, size exclusion and other RP-HPLC modes such as, ion-pair and micellar have been used to separate selected vanadium compounds. We will present a review that summarizes and critically analyzes the reported methods for analysis of vanadium salts and vanadium compounds in different sample matrices. We will compare various HPLC methods and modes including sample preparation, chelating reagents, mobile phase and detection methods. The comparison will allow us to identify the best analytical HPLC method and mode for measuring vanadium levels and what information such methods provide with regard to speciation and quantitation of the vanadium compounds.     

Novel anti-inflammatory and wound healing controlled released LDH-Curcumin nanocomposite via intramuscular implantation,in-vivo study

One of the most common problems in wounds is delayed healing and complications such as infection. Therefore, the need for novel materials accelerates the healing of wounds especially abdominal wounds after surgery besides high efficiency and safety is mandatory. The rate of wound healing, anti-inflammatory and biocompatibility of Zn-Al LDH (Zn-Al layer double hydroxide) alone and loaded with Curcumin (Zn-Al LDH/Curcumin) was screened via in-vivo assays through intramuscular implantation in rat abdominal wall with intact peritoneum cavity. The implanted drugs were formed through Curcumin loaded into LDH of Zn-Al with drug release of 56.78 ± 1.51% within 24 h. The synthesized nanocomposite was characterized by (TGA/DTA) thermal analysis, (XRD) X-ray diffraction, (FESEM) Field emission scanning electron microscopy, (HRTEM) high resolution transmission electron microscope, energy dispersive X-ray (EDX) and low-temperature N₂ adsorption, pore volume and average pore size distribution. The integrity of blood circulation, inflammatory signs, wound healing rate, capacity of tissue integration, antigenicity and composite biocompatibility, auto fluorescence ability of collagen bundles and the tensile strength of the muscle were assessed histopathologically after 7 and 30 days’ post-implantation. Excellent wound healing ability was achieved with shortest length between the wound gap edges and higher tensile strength of the muscle. Besides emit florescence very well followed by good healing and tensile muscles strength in Curcumin while very low strength with scar formation in Zn-Al LDH/Curcumin in both acute and chronic wound. No signs of inflammation in Curcumin & Zn-Al LDH. No vessels obstruction or bleeding observed in both Zn-Al LDH and Curcumin more than Zn-Al LDH/Curcumin and control which examined through candling. Good healing & infiltrated immune cells in same groups through histopathological examination. This work supports the anti-inflammatory, wound healing and biocompatibility of both LDH and Curcumin with living matter, increasing their biomedical applications in this era with safety and increasing efficacy with prolonged drug release.     

Quantitative analysis of delta9-tetrahydrocannabinol in preserved oral fluid by liquid chromatography-tandem mass spectrometry

A rapid and sensitive method for the analysis of delta9-tetrahydrocannabinol (THC) in preserved oral fluid was developed and fully validated. Oral fluid was collected with the Intercept, a Food and Drug Administration (FDA) approved sampling device that is used on a large scale in the U.S. for workplace drug testing. The method comprised a simple liquid-liquid extraction with hexane, followed by liquid chromatography-tandem mass spectrometry (LC-MS-MS) analysis. Chromatographic separation was achieved using a XTerra MS C18 column, eluted isocratically with 1 mM ammonium formate-methanol (10:90, v/v). Selectivity of the method was achieved by a combination of retention time, and two precursor-product ion transitions. The use of the liquid-liquid extraction was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Validation of the method was performed using both 100 and 500 MicroL of oral fluid. The method was linear over the range investigated (0.5-100 ng/mL and 0. 1-10 ng/mL when 100 and 500 microL, respectively, of oral fluid were used) with an excellent intra-assay and inter-assay precision (relative standard deviations, RSD <6%) for quality control samples spiked at a concentration of 2.5 and 25 ng/mL and 0.5 and 2.5 ng/mL, respectively. Limits of quantification were 0.5 and 0.1 ng/mL when using 100 and 500 microL, respectively. In contrast to existing GC-MS methods, no extensive sample clean-up and time-consuming derivatisation steps were needed. The method was subsequently applied to Intercept samples collected at the roadside and collected during a controlled study with cannabis.     

Thermal degradation behavior of radiation synthesized polydiallyldimethylammonium chloride

Thermogravimetric analysis (TGA) and differential scanning calorimetric (DSC) studies were carried out on gamma radiation synthesized polydiallyldimethylammonium chloride (PDADMAC). The polymer was found to undergo thermal degradation in two stages. The first stage showed a weight loss of 33% and the second stage showed a weight loss of 67%. The DSC thermogram shows two endothermic peaks corresponding to the two stages in the TG thermogram and the experimental enthalpy change associated with the first and second stages were 650 J g⁻¹ and 129.5 J g⁻¹, respectively. The nth-order kinetic parameters (order of the reaction, activation energy and the pre-exponential factor) were determined from a single dynamic DSC or thermogravimetric (TG) thermogram by the method of least square. Theoretical TG/differential thermogravimetric (DTG) and DSC thermograms derived from the calculated kinetic parameters were in good agreement with the experimental ones at the heating rate employed. However, the kinetic parameters determined using TG and DSC were different. This leads to the conclusion that the degradation mechanism could be complicated and may consists of a number of parallel or consecutive reactions. The glass transition temperature (T_g) of the polymer was found to be around 150 °C depending on the test method employed.     

螺栓连接的梁–弹簧模型及各齿承载分布

螺栓各齿承载分布严重不均,内外螺纹啮合的第一齿承载较大且齿根存在应力集中,易造成螺栓杆横断失效。本文通过对螺栓连接的受力变形分析,建立梁–弹簧模型,推导了理论模型的力学方程组,并基于此模型编程计算,求解得到螺栓连接件在使用过程中各齿承载的分布情况和齿根应力集中系数。最后进行有限元仿真,对比理论模型和有限元的结果,两者误差在工程可接受范围之内。研究表明,螺栓连接的组合梁–弹簧模型是合理有效的。

     

乐山泥岩的水土曲线和崩解特征试验研究

红层软岩的崩解性引发显著的软岩风化破裂现象,经常导致坡体不稳定、岩石崩落等不良地质现象。为深入理解泥岩的水土特征曲线（soil and water characteristic curve,SWCC）和浸水崩解特征,以乐山红层泥岩为例,采用滤纸法、浸水法等试验方法系统研究了泥岩的SWCC以及其在水中崩解的特征,构建了适合于该地区的SWCC模型,并讨论了浸水时间对泥岩崩解质量、颗粒级配的影响。结果表明：（1）泥岩的SWCC呈单峰曲线,随着含水率的减少,基质吸力增大。（2）通过与4种典型率定曲线的拟合比较,基质吸力拟合结果表现出良好的相关性（R²≥92%）,其中Fredlund &; Xing模型能够更准确地反映该地区泥岩的SWCC（R²=96%）。（3）浸水试验表明,0~6 h为快速崩解期,6~12 h为慢速崩解期,12 h后为长期崩解期。干湿交替浸水可以加速泥岩在亲水初期的崩解速率,但在最终崩解量方面与持续浸水基本一致。（4）浸水崩解后,颗粒粒径变化主要集中在2～20 mm范围内,级配曲线D₆₀,D₃₀,D₁₀和C_u值随着浸水时间的增大而减少,表明泥岩颗粒粒径随时间逐渐减小。（5）该泥岩耐崩解指数拟合公式为${y}$=1.17e^–0.22x,拟合度良好（R²≥99%）,根据I_d2=0.76判断该地区泥岩崩解性为弱~中等崩解性。该成果可为该地区泥岩的水土特性和崩解特性提供重要的定量数据支持,以及为该地区工程建设提供理论依据。

     

Spectroscopic assessment of biomolecular changes in Helicobacter pylori and Epstein–Barr virus co-infected gastric epithelial cells

Helicobacter pylori and Epstein–Barr Virus (EBV) are Group 1 carcinogens that can enhance gastric cancer progression. Bioactive substances extracted from plants can be effective therapeutic agents in cancer treatment. For example, Withania somnifera extract-WSE reduces the Gankyrin oncoprotein, which is upregulated in the presence of H. pylori and EBV. The various biochemical and metabolic changes upon 24 hrs post-infection followed by W. somnifera extract (WSE) treatment on gastric epithelial cells (AGS) can be studied using spectroscopic techniques. In the biomedical sciences, Raman and NMR spectroscopy have been extensively employed to interpret cellular alterations contributing to the onset of infection and the severity of gastric cancer. More specifically, alterations in cellular biochemical homeostasis are linked to the moieties of cholesterol, collagen, choline, carbohydrate, lipids, tyrosine, and phenylalanine. Further, we have found significantly elevated FWHM for carbohydrates, tumor associated protein, collagen, cholesterol, and cholesterol ester in the co-infection model. We also looked into the potential correlation between these molecules using molecular network analysis and found several related factors that can be modulated through biomolecular levels. These molecules are crucial in several physiological functions, including cell division, cell proliferation, apoptosis, necrosis, cell migration, and lipid transport. Our study paves the pathway to study H. pylori and EBV co-infection in human gastric epithelial cells and the therapeutic interventions of WSE in this scenario and highlights specific biomolecular alterations, which can be focused for further mechanistic investigations.     

结构光测量中的高精度相位误差补偿算法

在模拟分析投影仪伽马非线性对相位误差影响的基础上,提出一种直接分析投影光栅特征并建立相位误差查找表的算法.对相位误差进行补偿.该算法通过分析一组投射到标准白色平板上的光栅图像,确定光栅相位值与相位误差的对应关系,并量化存储在一个查找表中,测量过程中使用查找表对相位误差进行补偿.实验结果表明.该方法可大大降低由投影仪伽马非线性引起的相位误差,系统测量精度达到0.043 mm,比误差补偿前提高了5.6倍.     

Preparation of safe water–lipid mixed electrolytes for application in ion capacitor

Aqueous electrolytes are safe, economic, and environmentally friendly. However, they have a narrow potential window. On the other hand, organic electrolytes exhibit good thermodynamic stability but are inflammable and moisture sensitive. In this study, we prepared water–PEG–lipid ternary electrolytes(TEs). To combine the advantages of water, polyethylene glycol(PEG) and propylene carbonate(PC). The nonflammable mixed electrolytes exhibited a wide potential window of about 2.8 V due to the beneficial effects of PEG and PC. Using these TEs, a lithium manganate–active carbon ion capacitor could be operated at 2.4 V with an energy density of 32 Wh/kg, based on the total active electrode material(current density of 3.3 m A/cm~2). This value was significantly higher than that achieved using an aqueous electrolyte, thereby rationalizing the higher energy density.