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1.
A new trimethylamine amination polychloromethyl styrene nanolatex (TMAPL) and TMAPL coated capillary column (ccc‐TMAPL) were successfully prepared. The TMAPL coating was characterized with reversed steady EOF values of ca. ?16.8 × 10?5 cm2 V?1 s?1. It was applied to establish open‐tubular (OT) CEC and field‐amplified sample stacking (FASS) OT‐CEC methods for the determination of bromate in tap water. Compared to OT‐CEC, the LOD with FASS‐OT‐CEC was improved from 80 to 8 ng/mL. The developed FASS‐OT‐CEC method was practically used for the analysis of bromate in tap water samples with recoveries ranging from 93.6 to 103.5%.  相似文献   
2.
Hepatitis B core antigen (HBcAg) expressed in Escherichia coli is able to self‐assemble into large and small capsids comprising 240 (triangulation number T = 4) and 180 (triangulation number T = 3) subunits, respectively. Conventionally, sucrose density gradient ultracentrifugation and SEC have been used to separate these capsids. However, good separation of the large and small particles with these methods is never achieved. In the present study, we employed a simple, fast, and cost‐effective method to separate the T = 3 and T = 4 HBcAg capsids by using native agarose gel electrophoresis followed by an electroelution method (NAGE‐EE). This is a direct, fast, and economic method for isolating the large and small HBcAg particles homogenously based on the hydrodynamic radius of the spherical particles. Dynamic light scattering analysis demonstrated that the T = 3 and T = 4 HBcAg capsids prepared using the NAGE‐EE method are monodisperse with polydispersity values of ~15% and ~13%, respectively. ELISA proved that the antigenicity of the capsids was not affected in the purification process. Overall, NAGE‐EE produced T = 3 and T = 4 capsids with a purity above 90%, and the recovery was 34% and 50%, respectively (total recovery of HBcAg is ~84%), and the operation time is 15 and 4 times lesser than that of the sucrose density gradient ultracentrifugation and SEC, respectively.  相似文献   
3.
The phenomenon of peak area decrease due to high injection voltage (Vinj, e.g. 10–30 kV, 200–600 V/cm in the 50 cm capillary) was found in the analysis of very dilute DNA fragments (<0.2 mg/L) by using high‐sensitive electrokinetic supercharging‐CGE. The possibility of DNA cleavage in aqueous solution was suggested, in addition to the aggregation phenomenon that is already known. The analysis of intentionally voltage‐affected fragments (at 200 V/cm) also showed decreased peak areas depending on the time of the voltage being applied. Computer simulation suggested that a high electric field (a few kV/cm or more) could be generated partly between the electrode and the capillary end during electrokinetic injection (EKI) process. After thorough experimental verification, it was found that the factors affecting the damage during EKI were the magnitude of electric field, the distance between tips of electrode and capillary (De/c), sample concentration and traveling time during EKI in sample vials. Furthermore, these factors are correlating with each other. A low conductivity of diluted sample would cause a high electric field (over a few hundred volts per centimeter), while the longer De/c results in a longer traveling time during EKI, which may cause a larger degree of damage (aggregation and cleavage) on the DNA fragments. As an important practical implication of this study, when the dilute DNA fragments (sub mg/L) are to be analyzed by CGE using EKI, injection voltage should be kept as low as possible.  相似文献   
4.
The features of rock-forming elements determination in powder samples of peat sediments are considered. Based on theoretical calculations and experimental data, the mineralogical and particle size effects on the X-ray fluorescence intensity have been estimated. For routine analysis, powder rock samples are usually milled to a particle size of 10–60 μm. Theoretically, estimated variations of rock-forming elements analytical lines intensities in different minerals are up to 30%, and the particle size effect cannot be eliminated simultaneously for all rock-forming elements. Experimental estimation shows that the impossibility of the particle size distribution control can lead to significant variations in the intensities of the analytical lines (3%–18%) that is mainly corresponding to theoretical estimation. Fine milling allowed us to achieve an average particle size of fewer than 20 μm and reduce the measurement uncertainty by 1.5–2 times. 12 samples of peat sediments with organic matter content up to 70 wt% were analyzed by X-ray fluorescence analysis using different sample preparation techniques, as well as by certified methods. The accuracy of X-ray fluorescence analysis of peat sediments prepared as pressed pellets varies from 1.5 to 11 rel% depending on compound contents. It is more than for samples prepared as fused beads, however, the proposed method can be used to determine the variations of rock-forming elements contents in peat sediments where the content variations exceed the measurement uncertainty, and accuracy of analysis is sufficient for further paleoecological reconstructions.  相似文献   
5.
Advanced synchrotron radiation light is a powerful tool for archaeometry research. However, its applications to precious cultural relics, especially for color painting, have been hindered to some degree due to potential X-ray radiation damage. Compared to inorganic mineral pigments, organic binders in the painting are easier to be damaged by synchrotron radiation X-ray beam. The radiation damage effect of two typical painting samples, pure rabbit skin glue and the mixed sample of rabbit skin glue and zinc white, has been investigated by in situ time-resolved ED-XAS and IR combined techniques. The results show that the radiation damage effect of pure rabbit skin glue is more serious at low X-ray energy (7775 eV). The radiation damage effect of the mixed sample increases significantly due to more X-ray absorption by inorganic pigments. Furthermore, the radiation damage is more serious at the energy near Zn K-edge and is somewhat slight at higher energy (13,054 eV). These damages are more obvious from the point of view of protein secondary structures. The irradiation damage effects increase more rapidly at the beginning and are not linear with the irradiating time. The results indicate that synchrotron radiation damage can be reduced effectively by using X-ray energy far away from the X-ray absorption edge of the major element in the pigments during XRF, XRD and CT experiments, or by using time-resolved techniques such as QXAFS and ED-XAS during XAFS experiments.  相似文献   
6.
High-reflective multilayer laser coatings are widely used in advanced optical systems from high power laser facilities to high precision metrology systems. However, the real interface quality and defects will significantly affect absorption/scattering losses and laser induced damage thresholds of multilayer coatings. With the recent advances in the control of coating design and deposition processes, these coating properties can be significantly improved when properly engineered the interface and defects. This paper reviews the recent progress in the physics of laser damage, optical losses and environmental stability involved in multilayer reflective coatings for high power nanosecond near-infrared lasers. We first provide an overview of the layer growth mechanisms, ways to control the microstructures and reduce layer roughness, as well as the nature of defects which are critical to the optical loss and laser induced damage. Then an overview of interface engineering based on the design of coating structure and the regulation of deposition materials reveals their ability to improve the laser induced damage threshold, reduce the backscattering, and realize the desirable properties of environmental stability and exceptional multifunctionality. Moreover, we describe the recent progress in the laser damage and scattering mechanism of nodule defects and give the approaches to suppress the defect-induced damage and scattering of the multilayer laser coatings. Finally, the present challenges and limitations of high-performance multilayer laser coatings are highlighted, along with the comments on likely trends in future.  相似文献   
7.
The surface analysis of wood and wood products is becoming increasingly important for reasons ranging from the investigation of molecular constituents through to the optimization of industrial processes. As with any natural product, wood analysis is not straightforward, and this review aims to provide guidance for the successful surface analysis of wood by XPS and ToF-SIMS. Through example experiments, three themes are addressed relevant to obtaining meaningful results: considerations related to heterogeneity in the composition of wood (e.g., growth rings); the impact of the chemical removal of minor wood components known as extractives, and whether such a process is necessary; and the potential for misleading or erroneous results as a result of contamination occurring during sample preparation. In addition to discussing successful sample preparation approaches, the important role to be played by MVA in surface analysis is emphasized, particularly in the analysis of ToF-SIMS data. Examples of ToF-SIMS/MVA are provided that highlight the identification of contamination in sample preparation, the quantification of wood composition in terms of cellulose and lignin, and the indication of age of softwood samples. Through consideration of the complexities that influence wood surface analysis, the design and interpretation of consequential experiments become easier and more accurate.  相似文献   
8.
Current forensic DNA profiles are obtained based on analyses of PCR product sizes or DNA sequence polymorphisms. Sometimes routine forensic analysis using short tandem repeat (STR) generates unsuccessful DNA testing result if the biological sample encountered is excessively degraded and low-template DNA. Herein, a new six-color fluorescence labeling system, including 59 autosomal diallelic deletion or insertion polymorphisms (DIPs), 2 miniSTRs, 2 Y-chromosome DIPs, and 1 Amelogenin gene with the amplicon sizes of less than 200 bp, was self-developed. According to the validation guidelines for DNA analysis methods formulated by the Scientific Working Group on DNA Analysis Methods, the validation studies have also been carried out for the multiplex system. This novel panel possessed the features of strong stability, high sensitivity, and good specificity, which was especially suitable for the forensic degraded and mixed sample detections. The cumulative power of exclusion and cumulative matching probability of the system were 0.9999978 and 9.833E-28, respectively, in Han Chinese in Hunan, China. Moreover, this system will be an effective new tool that can be independently applied to forensic personal identification and paternity testing in the populations from the East Asia region, even from the South Asia, America, and Europe regions. The system can also contribute to population phylogenetic affinity and genetic structure analyses among different populations.  相似文献   
9.
Dynamic single-drop microextraction (SDME) was automatized employing an Arduino-based lab-made Cartesian robot and implemented to determine parabens in wastewater samples in combination with liquid chromatography–tandem mass spectrometry. A dedicated Arduino sketch controls the auto-performance of all the stages of the SDME process, including syringe filling, drop exposition, solvent recycling, and extract collection. Univariate and multivariate experiments investigated the main variables affecting the SDME performance, including robot-dependent and additional operational parameters. Under selected conditions, limit of detections were established at 0.3 µg/L for all the analytes, and the method provided linear responses in the range between 0.6 and 10 µg/L, with adequate reproducibility, measured as intraday relative standard deviations (RSDs) between 5.54% and 17.94%, (n = 6), and inter-days RSDs between 8.97% and 16.49% (n = 9). The robot-assisted technique eased the control of dynamic SDME, making the process more feasible, robust, and reliable so that the developed setup demonstrated to be a competitive strategy for the automated extraction of organic pollutants from water samples.  相似文献   
10.
New organotin(IV) derivatives containing the anionic ligands bis(3,5‐dimethylpyrazol‐1‐yl)dithioacetate [LCS2] and bis(3,5‐dimethylpyrazol‐1‐yl)acetate [LCO2] have been synthesized from reaction between (CH3)2SnCl2 and lithium salts of the ligands. Mononuclear complexes of the type {[LCX2](CH3)2SnCl} (X = S or O) have been obtained and fully characterized by elemental analyses and FT‐IR in the solid state and by NMR (1H, 13C and 119Sn) spectroscopy, conductivity measurements and electrospray ionization mass spectrometry in solution. The acute toxicity of new organotin(IV) derivatives on rat was studied, comparing their effect with those of dimethyltin chloride (CH3)2SnCl2. The comparison of LD50 of organotin(IV) complexes and (CH3)2SnCl2 administered intraperitoneally, as a single dose, evaluated in vivo on rats, showed that toxicity decreases as follows: (CH3)2SnCl2 > LCO2 > LCS2. The effect of these organotin(IV) complexes on DNA was evaluated in vitro and in vivo on rats treated with different doses of these compounds (1/20 LD50 and 1/100 LD50). The lymphocyte DNA status was assessed by the comet assay, a rapid and sensitive single‐cell electrophoresis technique, used to detect primary DNA damage in individual cells. After 36 h from the start of treatment the two new organotin(IV) derivatives induced a significant rise in comet assay parameters, indicating an increasing presence of damaged DNA. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   
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