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1.
A simple procedure for the synthesis of an important standard, isotopically enriched methylmercury, which is not commercially available, has been established successfully. The isotopically enriched standard synthesized is utilized in conventional isotope dilution mass spectrometry (IDMS), as well as in speciated IDMS (SIDMS), for determination of the true concentration of methylmercury in environmental samples. The CH3201Hg+ standard has been synthesized from commercially available 201HgO and tetramethyltin. The synthesis time required is 1 h at 60°C. The product is highly pure, yielding more than 90% as 201Hg in CH3201Hg+. Hazardous dimethylmercury does not occur during this synthesis procedure. The product synthesized was analyzed using high‐performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (ICP‐MS) and ICP‐MS alone in order to determine its concentration, isotopic composition and purity. The stability of the product was also evaluated for over 6 months and found to be stable at 4°C in the dark. The isotopically enriched methylmercury synthesized can be used in SIDMS and IDMS analyses as a standard. Copyright © 2003 John Wiley & Sons, Ltd. 相似文献
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Subbiah Meenakshisundaram RM. Sockalingam 《Journal of molecular catalysis. A, Chemical》2000,160(2):269-275
Catalytic activity of Os(VIII) in the oxidation of some twenty organic sulfides with sodium salt of N-chlorobenzenesulfonamide (CAB) has been investigated in alkaline (pH8.7) t-butanol–water (1:1 v/v) medium. Significant retarding influence of [OH−] on the reactivity is exhibited. The catalysed reaction is strongly accelerated in the presence of Hg(II). Imperfections are observed in the linear Hammett relationship in the case of –NO2 substituents. 相似文献
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Nano titanium dioxide (nTiO2), generally considered to be toxicologically inert, is manufactured in large quantities and extensively applied in consumer products. The small size and large surface area endow them with an active group or intrinsic toxicity. Advances in instrumentation are making Raman spectroscopy the tool of choice for an increasing number of (bio) chemical applications. One of the great advantages of this technique is its ability to provide information on the concentration, structure and interaction of biochemical molecules in their microenvironments within intact cells and tissues, non-destructively. Zebrafish (Danio rerio), one of the most important vertebrate model organisms used in developmental biology, are increasingly used in biomedical research, particularly as a model of human disease. In the present work, an attempt is made to study the effect of titanium dioxide, both nano and bulk, on the microenvironment of the liver tissues of Zebrafish using FT-Raman spectroscopy. The results of the present study suggest that TiO2 exposure demonstrate a marked influence on the microenvironments of the liver tissues of Zebrafish. A shift to a higher wavenumber and an increase in the intensity of the band at ∼1087 cm−1 in the TiO2 exposed tissues suggest that some of the conformational changes resulting from the alkali recovery process takes place due to TiO2 exposure. The decreased intensity ratio (I3220/I3400) observed in the titanium-exposed tissues suggests a decreased water domain size, which could be interpreted in terms of weaker hydrogen-bonded molecular species of water in the TiO2 exposed tissues. The observed shift of COO− bands to higher frequencies shows the disruption of salt bridges as a result of a change in the oppositely charged partners and due to the enhanced random coil conformation. The variation in the intensity ratio of the tyrosyl doublet (I858/I825) indicates variation in the hydrogen bonding of the phenolic hydroxyl group due to TiO2 exposure. The results further suggest that the microenvironments are greatly altered due to titanium nano exposure when compared to titanium bulk. In conclusion, the results indicate that FT-Raman spectroscopy might be a useful tool for rapid assessment of nano particle biological interactions. 相似文献
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One-step synthesis of labeled sugar nucleotides for protein O-GlcNAc modification studies by chemical function analysis of an archaeal protein 总被引:2,自引:0,他引:2
Herein we present the chemical function analysis of a recombinant sugar nucleotidyltransferase from the hyperthermophile Pyrococcus furiosus and its use in the one-pot synthesis of chloroacetyl- and alkyne-tagged analogues of uridinediphospho-N-acetylglucosamine (UDP-GlcNAc). The gene was originally annotated as a glucose-1-phosphate deoxythymidylyltransferase; however, kinetic analysis of a panel of sugar-1-phosphates with the protein shows that it is better described as a bifunctional protein that synthesizes UDP-GlcNAc from glucosamine-1-phosphate and acetyl coenzyme A (CoA). A new mass-spectrometry-based assay for the rapid analysis of the acyltransferase activity demonstrates that the enzyme can also accept cheaper truncated N-acetylcysteamine thioester substrates in place of the natural acetyl CoA. The enzyme can tolerate alkyne or chloride substitutions in the acyl moiety, thereby allowing the facile synthesis of tagged sugar nucleotides for future use in protein O-GlcNAc modification studies. 相似文献
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Mohammad Mizanur Rahman Kazuaki Ninomiya Chiaki Ogino Nobuaki Shimizu 《Ultrasonics sonochemistry》2010,17(4):738-743
A non-woven titanium dioxide (TiO2) fabric was applied to disinfection by ultrasound (US) irradiation, and the disinfection efficiency and lipid peroxidation of Escherichia coli (E. coli) cell membrane were evaluated to investigate the killing process. The addition of non-woven TiO2 fabric enhanced hydroxyl (OH) radical generation and disinfection efficiency. Judging from the disinfection experiments using glutathione or t-butanol as a radical scavenger, the OH radical played a major role in cell killing in sonodynamic disinfection with non-woven TiO2 fabric. Moreover, to understand the detailed killing process, damage to cell membrane was also evaluated using a diphenyl-1-pyrenylphosphine (DPPP) fluorescent probe, which detects the membrane’s lipid peroxidation. The addition of non-woven TiO2 fabric aggravated this peroxidation. This aggravation was caused by the OH radical according to an assay using a radical scavenger. From these results, it was concluded that non-woven TiO2 fabric as a sonocatalyst promoted peroxidation of the polyunsaturated phospholipid component of the lipid membrane initially and induced a major disorder in the E. coli cell membrane under US irradiation. 相似文献
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C McConville RM Kalin D Flood 《Rapid communications in mass spectrometry : RCM》1999,13(13):1339-1345
Current methods for stable oxygen isotopic (delta (18)O) analysis of soil water rely on separation of water from the soil matrix before analysis. These separation procedures are not only time consuming and require relatively large samples of soil, but also have been shown to introduce a large potential source of error. Current research at Queen's University Belfast is focused on using direct equilibration of CO(2) with the pore water to eliminate this extraction step using the automated Multiprep system and a Micromass Prism III isotope ratio mass spectrometer (IRMS). The findings of this research indicate the method is less time consuming, more reliable, and reproducible to within accepted limits (+/-0.1% per thousand delta (18)O). In this study the direct equilibration method is used to analyse delta (18)O tracer profiles in the unsaturated zone of field soils, concurrently with chloride tracer profiles, which can be used to assess infiltration rates and mechanisms through the unsaturated zone. Copyright 1999 John Wiley & Sons, Ltd. 相似文献
9.
RD Harris WS Baker Van Stipdonk MJ RM Crooks EA Schweikert 《Rapid communications in mass spectrometry : RCM》1999,13(14):1374-1380
A suite of keV polyatomic or 'cluster' projectiles was used to bombard unoxidized and oxidized self-assembled monolayer surfaces. Negative secondary ion yields, collected at the limit of single ion impacts, were measured and compared for both molecular and fragment ions. In contrast to targets that are orders of magnitude thicker than the penetration range of the primary ions, secondary ion yields from polyatomic projectile impacts on self-assembled monolayers show little to no enhancement when compared with monatomic projectiles at the same velocity. This unusual trend is most likely due to the structural arrangement and bonding characteristics of the monolayer molecules with the Au(111). Copyright 1999 John Wiley & Sons, Ltd. 相似文献
10.
Two dioctadecyl l-glutamic acid derivatives with amide and ester type bondings have been synthesized and immobilized from 3-aminopropyltrimethoxysilane (APS) grafted silica (Sil-APS) to be used in reversed-phase high-performance liquid chromatography (RP-HPLC). Subsequent studies showed that dioctadecyl-l-glutamide derivative (GLN) can self-assemble into highly ordered structures by forming three-dimensional fibrillar aggregates as observed in scanning and transmission electron microscopes (SEM and TEM). Variable temperature 1H NMR and FT-IR spectra of organogel revealed that the special aggregation morphology shown by GLN was stabilized by inter and or intra molecular hydrogen bonding among amide moieties. However, such ordered aggregated or self-assembled structures were not observed for the dioctadecyl-l-glutamate (GLU) derivative. The stationary phases Sil-GLN and Sil-GLU were characterized by DRIFT, elemental analysis, TGA, and 13C and 29Si CP-MAS NMR spectroscopic measurements. The chromatographic selectivity for both stationary phases was evaluated from the retention studies of different size and shape polycyclic aromatic hydrocarbons (PAHs). The chromatographic experiment for PAHs and geometrical isomers in RP-HPLC showed that Sil-GLN demonstrated extremely enhanced selectivity than Sil-GLU. The higher selectivity attributed by Sil-GLN has been brought by multiple π-π interactions among the π-electrons of the grafted organic phase and π-electrons of the guest PAHs molecules. Thermodynamic studies for linear and nonlinear PAHs revealed that the retention behavior does not change over a temperature range from 10 to 60 °C for both stationary phases. 相似文献