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1.
An ion‐pair reverse‐phase high performance liquid chromatographic method with UV–vis detection has been developed for the determination of total free iodine in rabbit plasma after vaginal administration of povidone–iodine (PVP‐I). Sample preparation was done by protein precipitation with acetonitrile in 96‐well format and aspirin was used as the internal standard. The 100 µL sodium thiosulfate solution (5 g L?1) was added to 100 µL plasma sample before protein precipitation, to convert the total free iodine in plasma to iodide (I?). Separation was performed on a C18 column (200 × 4.6 mm i.d., 5 µm). The mobile phase consisting of a mixture of water phase (containing 10 mmol L?1 18‐crown‐6 ether, 5 mmol L?1 octylamine and 5 mmol L?1 sodium dihydrogen phosphate, pH adjusted to 6.0 with phosphoric acid) and acetonitrile in the ratio 70:30 (v/v) was delivered isocraticly at a flow rate of 1.0 mL min?1. The method was sensitive with a lower limit of quantification of 0.005 µg mL?1, with good linearity (r2 > 0.9990) over the linear range of 0.005–2 µg mL?1. All the validation data, such as linearity, accuracy and precision, were within the required limits. The method was successfully applied to study the pharmacokinetic of PVP–I in rabbits after vaginal administration. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

2.
目的:建立刺激胰岛素分泌的新型降糖药物(-)-2 (S)-苄基-4-酮-4-(顺式-全氢化异吲哚-2-基)丁酸钙对映体的HPLC拆分方法。方法:采用Sumichiral OA-3300手性柱(250 × 4.6 mm I.D., 5 μm), 柱温35℃,以0.05 mol·L-1醋酸铵的甲醇溶液为流动相,检测波长为210 nm。结果:本品两对映体在22分钟内实现良好分离,分离度达3以上,S-异构体分别在0.028 ~ 5.6 μg mL-1和0.03 ~ 6.0 μg mL-1范围内线性关系良好,回归方程分别为:Y=1.32×103x-2.54 (r=0.9997)和Y=1.15×103x-1.78 (r=0.9998),最低检测限分别为0.15 ng和0.10 ng,方法精密度RSD低于1.0% (n=5)。结论:建立的对映体分离方法可用于本品光学异构体的质量控制。  相似文献   

3.
The voltammetric behavior of two genotoxic nitro compounds (4‐nitrophenol and 5‐nitrobenzimidazole) has been investigated using direct current voltammetry (DCV) and differential pulse voltammetry (DPV) at a polished silver solid amalgam electrode (p‐AgSAE), a mercury meniscus modified silver solid amalgam electrode (m‐AgSAE), and a mercury film modified silver solid amalgam electrode (MF‐AgSAE). The optimum conditions have been evaluated for their determination in Britton‐Robinson buffer solutions. The limit of quantification (LQ) for 5‐nitrobenzimidazole at p‐AgSAE was 0.77 µmol L?1 (DCV) and 0.47 µmol L?1 (DPV), at m‐AgSAE it was 0.32 µmol L?1 (DCV) and 0.16 µmol L?1 (DPV), and at MF‐AgSAE it was 0.97 µmol L?1 (DCV) and 0.70 µmol L?1 (DPV). For 4‐nitrophenol at p‐AgSAE, LQ was 0.37 µmol L?1 (DCV) and 0.32 µmol L?1 (DPV), at m‐AgSAE it was 0.14 µmol L?1 (DCV) and 0.1 µmol L?1 (DPV), and at MF‐AgSAE, it was 0.87 µmol L?1 (DCV) and 0.37 µmol L?1 (DPV). Thorough comparative studies have shown that m‐AgSAE is the best sensor for voltammetric determination of the two model genotoxic compounds because it gives the lowest LQ, is easier to prepare, and its surface can be easily renewed both chemically (by new amalgamation) and/or electrochemically (by imposition of cleaning pulses). The practical applicability of the newly developed methods was verified on model samples of drinking water.  相似文献   

4.
Yudum Tepeli  Ulku Anik 《Electroanalysis》2016,28(12):3048-3054
Three different Graphene‐Metallic (Graphene‐Me) nanocomposites – Graphene‐Silver (Graphene‐Ag), Graphene‐Gold (Graphene‐Au) and Graphene‐Platinum (Graphene‐Pt) nanocomposites – were prepared and characterized. The electrochemical performances of these nanocomposites were tested by incorporating them with glassy carbon paste electrode (GCPE) and used them in biofuel cells (BFC) and as amperometric xanthine biosensor transducers. Present work contains the first application of Graphene‐Au and Graphene‐Ag nanocomposite in BFCs and also first application of these Graphene‐Me nanocomposites in xanthine biosensors. Considering BFC, power and current densities were calculated as 2.03 µW cm?2 and 167.46 µA cm?2 for the plain BFC, 3.39 µW cm?2 and 182.53 µA cm?2 for Graphene‐Ag, 4.43 µW cm?2 and 230.15 µA cm?2 for Grapehene‐Au and 6.23 µW cm?2 and 295.23 µA cm?2 for Graphene‐Pt nanocomposite included BFCs respectively. For the amperometric xanthine biosensor linear ranges were obtained in the concentration range between 5 µM and 50 µM with the RSD (n=3 for 30 µM xanthine) value of 4.28 % for plain xanthine biosensor, 3 µM and 50 µM with the RSD (n=3 for 30 µM xanthine) value of 9.37 % for Graphene‐Ag, 5 µM to 20 µM with the RSD (n=3 for 5 µM xanthine) value of 9.00 % and 30 µM to 70 µM with the RSD (n=3 for 30 µM xanthine) value of 8.80 % for Grapehene‐Au and 1 µM and 70 with the the RSD (n=3 for 30 µM xanthine) value of 2.59 % for Grapehene‐Pt based xanthine biosensors respectively.  相似文献   

5.
Self‐assembly of the amphiphilic π‐conjugated carbenium ion ATOTA‐1+ in aqueous solution selectively leads to discrete and highly stable nanotubes or nanoribbons and nanorods, depending on the nature of the counterion (Cl? vs. PF6?, respectively). The nanotubes formed by the Cl? salt illustrate an exceptional example of a structural well‐defined (29±2 nm in outer diameter) unilamellar tubular morphology featuring π‐conjugated functionality and high stability and flexibility, in aqueous solution.  相似文献   

6.
A polymeric waveguide film was manufactured by spinning the materials on quartz substrate. Two‐photon‐initiated photopolymerization was carried out by tight‐focusing femtosecond laser pulses in the two‐mode planar waveguide. A typical index‐modulated grating of 2.5 × 2 mm areas without morphology was fabricated. The results show that peak‐to‐peak modulation depth of the surface profile of grating region was only about 7 nm. The diffraction efficiency (DE) of the grating with a spacing period 2 µm was 0.17% and the corresponding index modulation reached 5.7 × 10?3. Copyright © 2007 John Wiley & Sons, Ltd.  相似文献   

7.
Radiotracer batch ion‐exchange experiments were employed to investigate the uptake of 90Sr and 137Cs radioisotopes by various cation‐exchanged forms of a 30% cross‐linked macroporous 1‐vinyl‐2‐pyrrolidone–divinylbenzene cation‐exchange resin with 1.37 ml g?1 pore volume, 0.0232 µm pore diameter and 271.2 m2 g?1 surface area. The uptake of 90Sr and 137Cs was determined by taking liquid aliquots at various time intervals from solutions over solids. The volume‐to‐solid ratio was kept at 200. The results of kinetic experiments for the carrier‐free 90Sr and 137Cs were evident in all cationic forms of the resin. The percentage uptake and distribution coefficient Kd values with carrier (0.005 M SrCl2 and 0.01 M CsCl) concentrations were also determined, and the best results were obtained from the Li+ and H+ forms of the resin. Cerenkov counting (β?‐counting) was used to observe the initial and final radioactivity in the liquid phase. All the experiments were carried out at room temperature and the radioactivity in each case was corrected for the background counts. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

8.
A glassy carbon electrode coated the film of 4‐tert‐butyl‐1‐(ethoxycarbonylmethoxy)thiacalix[4]arene is designed for the determination of trace amounts of Hg2+. Compared with bare glassy carbon electrode, the modified electrode can improve the measuring sensitivity of Hg2+. Under the optimum experimental condition, the modified electrode in 0.1 mol L?1 H2SO4 + 0.01 mol L?1 KCl solution shows a linear voltammetric response in the range of 8.0 × 10?9 ~ 3.0 × 10?6 mol L?1 with detection limit 5.0 × 10?9 mol L?1 for Hg2+. The high sensitivity, selectivity, and stability of modified electrode also prove its practical application for a simple, rapid and economical determination of Hg2+ in water samples.  相似文献   

9.
A sensitive and selective method for the determination of Sb3+ based on the formation of its complexes with 8‐hydroxyquinoline (HQ) and 8‐hydroxyquinoline‐5‐sulfonic acid (HQS) is proposed. The best analytical conditions are: pH 5.4 and 2.2 for HQ and HQS, respectively; CHQ from 15.0 to 25.0 µmol L?1 and CHQS from 70.0 to 200.0 µmol L?1. The detection limits are 100.0 and 14.0 ng L?1 (tacc=30 s) for Sb3+ with HQ and HQS, respectively. The method using HQS as ligand has a 2.2‐fold higher sensitivity than that with HQ and the former was chosen for Sb3+ determination.  相似文献   

10.
A floating‐type low‐energy ion gun (FLIG) has been developed for high‐resolution depth profiling in ultrahigh vacuum (UHV). This UHV‐FLIG allows Ar+ ions of primary energy down to 50 eV to be provided with high current intensity. The developed UHV‐FLIG was sufficiently compact, being ~30 cm long, to be attached to a commercial surface analytical instrument. The performance of the UHV‐FLIG was measured by attaching it to a scanning Auger electron microprobe (JAMP‐10, Jeol), the base pressure of which in the analysis chamber was ~1 × 10?7 Pa. The vacuum condition of ~5 × 10?6 Pa was maintained during operation of the UHV‐FLIG without a differential pumping facility. Current density ranged from 41 to 138 µA cm?2 for Ar+ ions of primary energy 100–500 eV at the working distance of 50 mm. This ensures a sputtering rate of ~10 nm h?1 with 100 eV Ar+ ions for Si, leading to depth profiling of high resolution in practical use. Copyright © 2003 John Wiley & Sons, Ltd.  相似文献   

11.
On the basis of the principle of combination of active groups, a series of novel N‐(4‐([2,2′:5′,2′′‐terthiophen]‐5‐yl)‐2‐methylbut‐3‐yn‐2‐yl) benzamide derivatives were designed, synthesized and systematically evaluated for their antiviral activity against tobacco mosaic virus (TMV). The bioassay results showed that most of these compounds displayed good anti‐TMV activity, and some of them exhibited higher antiviral activity than commercial Ningnanmycin. Especially, compound 8e with excellent anti‐TMV activity (inactivation activity, 92.3%/500 µg·mL?1; curative activity, 85.7%/500 µg·mL?1 and protection activity, 64.7%/500 µg·mL?1) emerged as a potential inhibitor of plant virus TMV. Quantitative structure‐activity relationship studies proved that the van der Waals volume (V) and electronic parameter (∑(∑σo+σp) and ∑σm) for the substituent R1 were very important for antiviral activities in this class of compounds.  相似文献   

12.
Gold nanoparticles of different morphologies have been synthesized on a silica‐based organic‐inorganic hybrid material for catalytic applications. The gold nanoparticles formations proceed through in situ chemical reduction of the AuCl4? anions previously adsorbed on 3‐(1‐imidazolyl)propyl‐silsesquioxane, which plays the role of substrate and stabilizer. Two distinct reducing agents, sodium citrate and sodium borohydride, were employed to generate gold nanoparticles of different sizes. UV‐vis diffuse reflectance as well as transmission electron microscopy were employed to evaluate the particle’s morphology. Modified carbon paste electrodes were prepared from these materials and their electrochemical behavior investigated using potassium ferrocyanide and 4‐nitrophenol as redox model compounds. Both AuNPs‐modified electrodes decreased the overpotential of 4‐nitrophenol reduction by around 90 mV compared to the unmodified electrode as evidenced by cyclic voltammetry experiment. However, the smaller diameter particles (borohydride‐reduced) produced more significant catalytic effect as a consequence of their large surface area. Regarding the sensing parameters, the sensitivity is higher for the borohydride‐reduced AuNPs while the values of limit of detection are of the same order of magnitude. Thus, the detection limit and sensitivity are 70.0±0.6 nM and 187 µA/mM for the citrate‐reduced AuNPs; and 75.0±2.2 nM and 238 µA/mM for the borohydride‐reduced AuNPs.  相似文献   

13.
A series of 2‐(arylimino)benzylidene‐9‐arylimino‐5,6,7,8‐tetrahydrocyclohepta[b] pyridyliron(II) chlorides was synthesized and characterized using FT‐IR and elemental analysis, and the molecular structures of complexes Fe3 and Fe4 have been confirmed by the single‐crystal X‐ray diffraction as a pseudo‐square‐pyramidal or distorted trigonal‐bipyramidal geometry around the iron core. On activation with methylaluminoxane (MAO) or modified methylaluminoxane (MMAO), all iron precatalysts exhibited high activities toward ethylene polymerization with a marvelous thermo‐stability and long lifetime. The Fe4 /MAO system showed highest activity of 1.56 × 107 gPE·mol?1(Fe)·h?1 at 70 °C, which is one of the highest activities toward ethylene polymerization by iron precatalysts. Even up to 80 °C, Fe3 /MAO system still persist high activity as 6.87 × 106 g(PE)·mol?1(Fe)·h?1, demonstrating remarkable thermal stability for industrial polymerizations (80–100 °C). This was mainly attributing to the phenyl modification of the framework of the iron precatalysts. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55 , 830–842  相似文献   

14.
Monolithic columns were synthesized inside 1.02 mm internal diameter fused‐silica lined stainless‐steel tubing. Styrene and butyl, hexyl, lauryl, and glycidyl methacrylates were the functional monomers. Ethylene glycol dimethacrylate and divinylbenzene were the crosslinkers. The glycidyl methacrylate polymer was modified with gold nanoparticles and dodecanethiol (C12). The separation of alkylbenzenes was investigated by isocratic elution in 60:40 v/v acetonitrile/water. The columns based on polystyrene‐co‐divinylbenzene and poly(glycidyl methacrylate)‐co‐ethylene glycol dimethacrylate modified with dodecanethiol did not provide any separation of alkyl benzenes. The poly(hexyl methacrylate)‐co‐ethylene glycol dimethacrylate and poly(lauryl methacrylate)‐co‐ethylene glycol dimethacrylate columns separated the alkyl benzenes with plate heights between 30 and 60 μm (50 μL min?1 and 60°C). Similar efficiency was achieved in the poly(butyl methacrylate)‐co‐ethylene glycol dimethacrylate column, but only at 10 μL min?1 (0.22 mm s?1). Backpressures varied from 0.38 MPa in the hexyl methacrylate to 13.4 MPa in lauryl methacrylate columns (50 μL min?1 and 60°C). Separation of proteins was achieved in all columns with different efficiencies. At 100 μL min?1 and 60°C, the lauryl methacrylate columns provided the best separation, but their low permeability prevented high flow rates. Flow rates up to 500 μL min?1 were possible in the styrene, butyl and hexyl methacrylate columns.  相似文献   

15.
《Analytical letters》2012,45(6):1171-1185
Abstract

A simple and selective method based on a sodium dodecyl sulfate (SDS)–coated chromosorb P modified by 2‐mercaptobenzoxazole (MBO) has been developed to selectively separate and concentrate ultra trace amounts of mercury(II) ions for its highly sensitive measurement by cold vapor atomic absorption spectrometry (CVAAS).

The mercury ions were adsorbed quantitatively on SDS‐coated chromosorb due to its complexation with MBO, while the retained Hg2+ ions were then stripped from the column with minimal amounts of 2 M nitric acid in acetone. The eluting solution was sent to CV‐AAS for evaluating Hg2+ ion content and results indicate that the calibration curve was linear for Hg2+ ion in the range of 0.05–85.6 ng mL?1 and 0.09–9.6 µg mL?1 of Hg2+ ions. Maximum capacity of the SDS‐coated chromosorb modified with 40 mg of the ligand was found to be 498±30 µg of mercury(II), the limit of detection was 0.01 ng mL?1, and enrichment factors were about 300, which make it suitable it for dilute solution analysis. The method was successfully applied to the determination of Hg2+ ion content in real samples.  相似文献   

16.
The γ‐initiated reversible addition–fragmentation chain transfer mediated free‐radical graft copolymerization of styrene and m‐isopropenyl‐α,α′‐dimethylbenzyl isocyanate (TMI) from a polypropylene (PP) solid phase was performed with cumyl phenyldithioacetate (CPDA) as the chain‐transfer agent. The initial CPDA concentration was 8 × 10?3 mol L?1. Polymerizations were performed with a dose rate of 0.18 kGy h?1 at the ambient temperature. Initial comonomer mixtures with 15, 30, and 50 mol % TMI were used. Depending on the amount of TMI in the initial comonomer mixture, the plot of the grafting ratio versus the time showed two grafting regimes (for 15 and 50 mol % TMI) or one (for 30 mol % TMI). Scavenger lanterns with 15 and 50 mol % TMI featured two isocyanate loading regimes, the second with higher loading capacities. The scavenger lanterns with 30 mol % TMI showed a linear loading capacity over the full grafting ratio. A maximum loading capacity of 110 μmol per scavenger lantern was achieved with 50 mol % TMI at a grafting ratio of approximately 60 wt %. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 857–864, 2006  相似文献   

17.
Six new 1,3‐diorganylimidazolidin‐2‐ylidene (NHC) gold(I) complexes of the type [Au(NHC)2]+ (1–6), were synthesized by reacting [AuCl(PPh)3] with 1,3‐dimesitylimidazolidin‐2‐ylidene or bis(1,3‐dialkylimidazolidin‐2‐ylidene). The complexes 1–6 were fully characterized by elemental analyses and spectroscopic data. The placement of mesityl or para‐substituted benzyl groups on the nitrogen atoms of the ring of the complexes leads to the particularly active antibacterial agents evaluated in this work. It is worth noting that the p‐methoxybenzyl derivative (2) inhibited the growth of Pseudomona aeruginosa, Staphylococcus epidermidis, Staphylococcus aureus and Enterococcus faecalis with minimum inhibitory concentration (MIC) values of 3.12 µg ml?1, 6.25 µg ml?1, 3.12 µg ml?1 and 3.12 µg ml?1 respectively. In contrast, the analogous p‐dimethylaminobenzyl derivative (3) is effective only against Escherichia coli (MIC = 3.12 µg ml?1). Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

18.
A LC‐MS/MS method for the determination of a hydrophilic paclitaxel derivative 7‐xylosyl‐10‐deacetylpaclitaxel in rat plasma was developed to evaluate the pharmacokinetics of 7‐xylosyl‐10‐deacetylpaclitaxel in the rats. 7‐Xylosyl‐10‐deacetylpaclitaxel and docetaxel (IS for 7‐xylosyl‐10‐deacetylpaclitaxel) were extracted from rat plasma with acetic ether and analyzed on a Hypersil C18 column (4.6 × 150 mm i.d., particle size 5 µm) with the mobile phase of ACN/0.05% formic acid (50:50, v/v). The analytes were detected using an ESI MS/MS in the multiple reaction monitoring mode. The standard curves for 7‐xylosyl‐10‐deacetylpaclitaxel in plasma were linear (>0.999) over the concentration range of 2.0–1000 ng/mL with a weighting of 1/concentration2. The method showed a satisfactory sensitivity (2.0 ng/mL using 50 µL plasma), precision (CV ≤ 10.1%), accuracy (relative error ?12.4 to 12.0%), and selectivity. This method was successfully applied to the pharmacokinetic study of 7‐xylosyl‐10‐deacetylpaclitaxel in rat plasma after intravenous administration of 7‐xylosyl‐10‐deacetylpaclitaxel to female Wistar rats. Copyright © 2008 John Wiley & Sons, Ltd.  相似文献   

19.
A simple and cost‐effective HPLC method was established for quantification of 5‐hydroxyeicosatetraenoic acid (5‐HETE) in human lung cancer tissues. 5‐HETE from 27 patients' lung cancer tissues were extracted by solid‐phase extraction and analyzed on a Waters Symmetry C18 column (4.6 × 250 mm, 5 µm) with a mobile phase consisting of methanol, 10 mm ammonium acetate, and 1 m acetic acid (70:30:0.1, v:v:v) at a flow rate of 1.0 mL/min. The UV detection wavelength was set at 240 nm. The calibration curve was linear within the concentration range from 10 to 1000 ng/mL (r2 > 0.999, n = 7), the limit of detection was 1.0 ng/mL and the limit of quantitation was 10.0 ng/mL for a 100 µL injection. The relative error (%) for intra‐day accuracy was from 93.14 to 112.50% and the RSD (%) for intra‐day precision was from 0.21 to 2.60% over the concentration range 10–1000 ng/mL. By applying this method, amounts of 5‐HETE were quantitated in human lung cancer tissues from 27 human subjects. The established HPLC method was validated to be a simple, reliable and cost‐effective procedure that can be applied to conduct translational characterization of 5‐HETE in human lung cancer tissues. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

20.
A novel highly sensitive electrochemiluminescence (ECL) detection protocol for mercury(II) ions was developed. Based on the strong and stable thymine? thymine mismatches complexes coordination chemistry, mercury(II) ions can specifically bind to a designed DNA strand, leading to the release of the complimentary DNA strand. The released DNA strand was then captured by magnetic beads modified with specific DNA, and then through the formation of DNA‐linked luminol‐Au nanoparticles (NPs) superstructure, a specific ECL system for mercury(II) ions was developed. Using 3‐aminopropyl‐triethoxysilane as an effective enhancer, the ECL system can detect Hg2+ ion within a linear range from 2.0×10?10 mol L?1 to 2.0×10?8 M, with a detection limit as low as 1.05×10?10 M (3σ). Moreover, this ECL system is highly specific for Hg2+, without interference from other commonly coexisted metal ions, and it can be used for the analysis of real samples.  相似文献   

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