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1.
Abstract

The chemical composition of Tussilago farfara L. essential oil from the Saguenay-Lac-St-Jean region of Quebec, Canada was analyzed by gas chromatography–flame ionisation detector (GC-FID) and gas chromatography–mass spectrometry (GC-MS), and the antibacterial activity of the oil was tested against Escherichia coli and Staphylococcus aureus. Forty-five (45) compounds were identified from the GC profile. The main components were 1-nonene (40.1%), α-phellandrene (26.0%) and ρ-cymene (6.6%). The essential oil demonstrated antibacterial activity against E. coli (MIC50 = 468 µg·mL?1; MIC90 = 6869 µg·mL?1) and S. aureus (MIC50 = 368 µg·mL?1; MIC90 = 773 µg·mL?1). Dodecanoic acid was found to be active against both bacteria having a MIC50 and MIC90 of 16.4 µg·mL?1 and 95 µg·mL?1, respectively for E. coli and a MIC50 and MIC90 of 9.8 µg·mL?1 and 27.3 µg·mL?1, respectively for S. aureus. In addition, 1-decene and (E)-cyclodecene were also found to be active against E. coli.  相似文献   

2.
A miniaturized flow-injection-analysis system constructed from glass and polydimethylsiloxane was employed for the determination of ammonium in river water. The sample was filtered and delivered to the reactor chip electro-osmotically using a disposable fritted capillary, while reagents were delivered to the system by gravity. Ammonia was mixed with the hypochlorite, to form a monochloramine. Once the alkaline luminol (3-aminophthalhydrazide) was delivered to the system, it was oxidized by the unconsumed hypochlorite emitting a bright blue light (λ max?~?440?nm) that was detected using a miniaturized photomultiplier tube (PMT) located directly under the chip. The calibration model for ammonium standards was linear up to 0.1?µg?mL?1 (y?=??8.96x?+?1.02; correlation coefficient, r 2?=?0.9715) over a working range of 0.0–0.5?µg?mL?1. A detection limit of 10?±?6?µg?mL?1 was achieved with a precision value of (RSD ≤ 6.4%), for n?=?5. A direct and standard addition method were used to determine the concentration of ammonium in a river-water sample (from the Humber Estuary, UK) which was found to be 0.075?±?0.005?µg?mL?1, with a precision value of (RSD?≤?3.7%), for n?=?9. The results obtained showed good agreement with the average concentration 0.065?µg?mL?1 (provided by the local environmental agency), for the analysis of ammonia at different sample points on the estuary.  相似文献   

3.
A rapid, simple, and reliable competitive immunoassay was developed for measurement of lead ions Pb(II) in environmental samples. Avian antibodies were produced against Pb(II). Since lead ions are too small to elicit an immune response, the metal was coupled to protein carrier Bovine serum albumin (BSA) using a bifunctional chelator 1-(4-isothiocyanobenzyl) ethylenediamine N,N,N′,N′-tetra acetic acid (ITCBE). Poultry birds (layers) were immunised with this Pb(II)–ITCBE–BSA immunoconjugate and the avian antibodies (IgY) isolated from egg yolk recognised Pb(II)-ITCBE complexes as capture reagent and a Pb(II)–ITCBE conjugate of Alkaline phosphatase as an enzyme label. Antibody reaction was optimised for different concentrations of antigen and antibody dilutions. Cross reactivity with other metals were below 1% in competitive ELISA. The IC50 value of this avian antibody was 0.19?µg?mL?1. The detection range and the detection limit were 0.02–1000?µg?mL?1and 0.2?µg?mL?1, respectively.  相似文献   

4.
In the search for antitumor active metal complexes several ruthenium complexes have been reported to be promising. A series of mononuclear Ru(II) complexes, [Ru(T)2(S)]2+, where T?=?2,2′-bipyridine/1,10-phenanthroline and S?=?CH3-bitsz, Cl-bitsz, Br-bitsz, tmtsz, dmtsz, have been prepared and characterized by UV-Vis, IR, 1H-NMR, FAB-mass spectroscopy, and elemental analysis. The complexes were subjected to in vivo anticancer activity against a transplantable murine tumor cell line Ehrlich's ascitic carcinoma (EAC) and in vitro cytotoxic activity against human cancer cell line Molt 4/C8, CEM, and murine tumor cell line L1210. Ruthenium complexes showed promising biological activity especially in decreasing tumor volume and viable ascitic cell counts. Treatment with these complexes prolonged the life span of EAC-tumor-bearing mice by 10–48%. In vitro evaluation of these ruthenium complexes revealed cytotoxic activity from 0.21 to 24?µmol?L?1 against Molt 4/C8, 0.16–19?µmol?L?1 against CEM, and 0.75–32?µmol?L?1 against L1210 cell proliferation, depending on the nature of the compound.  相似文献   

5.
《Analytical letters》2012,45(12):1999-2013
Abstract

A simple, rapid, selective, and sensitive method for the derivative spectrophotometric determination of Hg(II) and its simultaneous determination in the presence of Zn(II) using 2‐(5‐bromo‐2‐pyridylazo)‐5‐diethylaminophenol in the presence of cetylpyridinium chloride, a cationic surfactant, has been developed. The molar absorption coefficient and analytical sensitivity of the 1∶1 Hg(II) complex at 558 nm (λmax) are 5.78×104 L mol?1 cm?1 and 0.67 ng mL?1, respectively. The detection limit of Hg(II) is 1.40×10?2 ng mL?1, and Beer's law is valid in the concentration range 0.05–2.40 µg mL?1. Overlapping spectral profiles of Hg(II) and Zn(II) complexes in zero‐order mode interfere in their simultaneous determination. However, 0.10–2.00 µg mL?1 of Hg(II) and 0.065–0.650 µg mL?1 of Zn(II), when present together, can be simultaneously determined at zero cross point of the derivative spectrum, without any prior separation. The relative standard deviation for six replicate measurements of solutions containing 0.134 µg mL?1 of Hg(II) and 0.620 µg mL?1 of Zn(II) is 1.72 and 1.47%, respectively. The proposed method has successfully been evaluated for trace level simultaneous determination of Hg(II) and Zn(II) in environmental samples.  相似文献   

6.
[M(HL)2] complexes (M = Co(II) (1), Ni(II) (2), and Cu(II) (3); H2L = 4-hydroxybenzoic[(5-nitro-2-furanyl)methylene]hydrazide acid, nifuroxazide) were synthesized, characterized (by elemental analysis, TG, IR, UV–vis., EPR, magnetic, and conductance measurements) and tested for their antimicrobial activities. H2L is a mono-negative bidentate ligand via hydrazone N and C–O? forming intermediate complexes between tetrahedral and square-planar geometries (“flattened” tetrahedron, D2d symmetry) for 1 and 2, as well as square-planar for Cu(II) complex 3. Natural bond orbital analysis revealed that the interaction of oxygen with metal ion is the main factor which determines the stability of 13 as the binding energy decreases with an increase in the M–O bond length. Time-dependent density functional theory calculations were carried out to understand the electronic transitions in related experimental observations. The reduction potential values of the nitro group are affected by the metal center. Ni(II) complex 2 displayed the highest activity among the tested complexes against Escherichia coli with a MIC50 value of 0.098 μmol mL?1 compared with 0.131 (1) and 0.117 μmol mL?1 (3).  相似文献   

7.
《Analytical letters》2012,45(10):1471-1478
Abstract

A simple, rapid, and sensitive chemiluminescence method for the determination of colistin (Polymyxin E), a cyclic polypeptide with antibiotic effect produced by certain strains of Bacillus polymyxa, has been developed by combining a flow-injection technique and the bacteria's sensitizing effect on the chemiluminescence reaction between sulfite and acidic permanganate. The optimum conditions for chemiluminescence emission were established. The chemiluminescence was proportional to the log of concentration of colistin over the range 4–100 µg mL?1 (3.5–87 µM). The detection limit was 1.2 µg mL?1 (1.0 µM) of colistin. The method has been satisfactorily used for the determination of colistin in pharmaceuticals.  相似文献   

8.
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   

9.
Stoichiometric reactions of 4,4'-diacetylcurcumin ( HL ) with series of transition metal ions, namely Fe3+, Co2+, Ni2+ and Zn2+, in methanol result in the corresponding homoleptic metal complexes. All the obtained complexes were characterized by elemental analysis, high resolution mass spectrometry, IR spectroscopy, magnetic moment and single-crystal X-ray diffraction. Structural analyses are unprecedentedly performed for the FeIII, CoII, and NiII complexes and reveal octahedral mononuclear complexes with the compositions [Fe(L)3] and [M(L)2(MeOH)2] (M = Co2+, Ni2+, Zn2+) for trivalent and divalent metal ions, respectively. In all complexes, the deprotonated ligands serve as monoanionic and bidentate ligands with (O,O)-chelating β-diketonate moieties. The free ligand HL exhibits considerable antiproliferative effects for the human MCF-7 breast and HepG2 liver cancer cells with IC50 values of 20.91 ± 2.16 μg · mL–1 and 12.85 ± 1.85 μg · mL–1, respectively. The CoII and ZnII complexes with IC50 values in the range of 14.53–20.80 μg · mL–1 for MCF-7 breast and 8.48–10.68 μg · mL–1 for HepG2 liver cancer cells show stronger antiproliferative effects than HL, the FeIII and NiII complexes cause weaker reductions of the growth of the two tested cancer cell lines.  相似文献   

10.
Two metal complexes, [NiII(mscinn)2(pda)2] (1) and [CdII(mscinn)2(dmeda)2·2H2O] (2) (mscinn?=?4-methylsulfonyl cinnamate, pda?=?propane-1,3-diamine, dmeda?=?N′,N′-dimethylethane-1,2-diamine), were synthesized by reacting 4-methylsulfonyl cinnamate with the diamines and metal salts. Their structures were determined by single-crystal X-ray diffraction analysis. Crystal parameters of 1: C26H38N4NiO8S2, M?=?657.43, monoclinic, P21/c, a?=?16.6123(8)?Å, b?=?8.5956(4)?Å, c?=?11.2047(5)?Å, β?=?107.423(1)°, V?=?1526.54(12)?Å3, Z?=?2, D calcd?=?1.430?g?cm?3, F(000)?=?692, μ?=?0.825?mm?1, R 1?=?0.0257, wR 2?=?0.0669. Crystal data of 2: C28H42CdN4O8S2?·?2(H2O), M?=?775.24, monoclinic, P21/c, a?=?9.8278(4)?Å, b?=?11.6611(5)?Å, c?=?15.3972(7)?Å, β?=?96.195(1)°, V?=?1754.26(13)?Å3, Z?=?2, D calcd?=?1.468?g?cm?3, F(000)?=?804, μ?=?0.798?mm?1, R 1?=?0.0299, wR 2?=?0.0770. Antimicrobial activities for 1 and 2 against Escherichia coli, Pseudomonas putida, Bacillus subtilis, and Bacillus cereus had better antibacterial activity than their parent carboxylic acid against Gram-positive bacteria (B. subtilis and B. cereus). The cadmium complex of the cinnamate displayed high inhibitory activity with an MIC value of 5?µg?mL?1 against P. putida, while the nickel complex also exhibited good inhibitory potency with an MIC value of 5?µg?mL?1 against B. subtilis.  相似文献   

11.
Two liquid-phase microextraction (LPME) approaches, static direct-immersed single-drop microextraction (DI-SDME) and continuous-flow microextraction (CFME), were used to extract methomyl in water samples and their respective extraction efficiencies were compared. Several important parameters affecting extraction efficiency such as the type of extraction solvent, solvent drop volume, stirring speed or flow rate, extraction time and salt concentration were optimised. The optimised conditions were as follows: 3.0-µL tetrachloroethane (C2H2Cl4) as the extraction solvent, 15% NaCl (w/v), 15 min extraction time and stirring speed at 600 rpm for DI-SDME; 3.5-µL C2H2Cl4 as the extraction solvent, 15% NaCl (w/v), 21 min extraction time and flowing rate at 0.8 mL min?1 for CFME. Under the previous optimal conditions, the linear range, detection limit (S/N = 3) and precision (RSD, n = 6) were 5.0-5000 ng mL?1, 1.5 ng mL?1, 6.9% for DI-SDME, and 4.0–10000 ng mL?1, 2.5 ng mL?1, 4.6% for CFME, respectively. Lake and river water samples were successfully analysed by DI-SDME and CFME. The result demonstrated that both SDME and CFME techniques are simple, low cost and amity to environment. As a result, the two approaches have tremendous potential in trace analysis of methomyl in natural waters.  相似文献   

12.
A miniaturized flow-injection analysis system constructed from a glass base plate and polydimethylsiloxane (PDMS) top plate was employed for the determination of iron in river water. Two designs were investigated, one utilizing a syringe pump and the other utilizing EOF pumping with a mini-filtration system incorporated. The syringe pump system was used to optimize the analytical method on chip, where the pump was used to deliver both the analyte and the reagents to the reactor chip. The highly sensitive chemiluminescence reaction between alkaline luminol (3-aminophthalhydrazide) and 0.1?M of hydrogen peroxide (H2O2) in the presence of iron(II) was utilized. The bright blue light (λ max?~?440?nm) emitted was detected using a miniaturized photomultiplier tube interfaced directly under the chip. The light intensity signals were recorded, and the corresponding concentration of iron(II) concentration was determined. The calibration for iron(II) standards was linear up to 0.75?µg?mL?1 (y?=?5.7839x?+?0.0378, r2 ?=?0.9939) with a precision value of up to 3.72% RSD, for n?=?3. The limits of detection (blank?+?3s y/x) were found to be 28?ng?mL?1. The system which utilized EOF pumping and incorporated a minifiltration unit provided a linear calibration for 0–5?µg?mL?1 (y?=?3.316x?+?0.1831; correlation coefficient, r 2?=?0.9996) over a working range of 0.0–0.5?µg?mL?1. This system provided lower limits of detection 5.1?ng?mL?1 and better repeatability (%RSD less than 0.5% for n?=?4), but problems occurred with the mini-filtration system at higher iron(II) concentrations. The EOF pumping system provided slightly higher results for the concentration of iron(II) in the Humber estuary (0.058?µg?mL?1), but these results were in line with the results expected by the Environment Agency.  相似文献   

13.
The polymeric precursor [RuCl2(CO)2]n reacts with the ligands, P∩P (a, b) and P∩O (c, d), in 1:1 M ratio to generate six-coordinate complexes [RuCl2(CO)2(?2-P∩P)] (1a, 1b) and [RuCl2(CO)2(?2-P∩O)] (1c, 1d), where P∩P: Ph2P(CH2)nPPh2, n = 2(a), 3(b); P∩O: Ph2P(CH2)nP(O)Ph2, n = 2(c), 3(d). The complexes are characterized by elemental analyses, mass spectrometry, thermal studies, IR, and NMR spectroscopy. 1a1d are active in catalyzed transfer hydrogenation of acetophenone and its derivatives to corresponding alcohols with turnover frequency (TOF) of 75–290 h?1. The complexes exhibit higher yield of hydrogenation products than catalyzed by RuCl3 itself. Among 1a1d, the Ru(II) complexes of bidentate phosphine (1a, 1b) show higher efficiency than their monoxide analogs (1c, 1d). However, the recycling experiments with the catalysts for hydrogenation of 4-nitroacetophenone exhibit a different trend in which the catalytic activities of 1a, 1b, and 1d decrease considerably, while 1c shows similar activity during the second run.  相似文献   

14.
Three new propanedithiolate-type iron–sulfur complexes containing tris(aromatic)phosphine ligands, [{(μ-SCH2)2CH2}Fe2(CO)5L] (L?=?P(PhOMe-p)3, 1; P(PhMe-p)3, 2; P(PhF-p)3, 3), have been prepared through carbonyl substitution in the presence of Me3NO. The new complexes 1–3 were characterized by elemental analysis, IR, 1H, 13C{1H}, and 31P{H} NMR spectra. The molecular structures of 1–3 were unequivocally determined by single crystal X-ray diffraction, in which the tris(aromatic)phosphine coordinated to Fe resides in an apical position of the pseudo-square-pyramidal geometry. IR spectroscopy and X-ray crystallographic analysis for 1–3 have indicated that the highly electron rich tris(aromatic)phosphine ligands (where the corresponding electron-donating abilities display the following order of P(PhOMe-p)3?>?P(PhMe-p)3?>?P(PhF-p)3) result in a considerable red shift of the CO-stretching frequencies and a clear change of the Fe–Fe bond distances in 1–3.  相似文献   

15.
A N-donor containing carboxylic ligand, 5-(pyridin-4-yl)isophthalic acid (H2L), was applied to construct two new coordination polymers [Cd(L)(DMF)] n (1, DMF?=?N,N-dimethylformamide) and {[Co(L)(H2O)2]?·?0.5CH3OH?·?1.5H2O} n (2) under different conditions. The complexes were characterized by IR, elemental, and thermogravimetric analyses, powder and single crystal X-ray diffraction. In 1 each L2? links four CdII to form a 3-D framework, while in 2 each L2? connects three metals to form a 2-D layer structure, which is further connected together by hydrogen bonds to form a 3-D architecture. The thermal stability of the complexes and the photoluminescence of 1 were investigated.  相似文献   

16.
A series of structurally similar dinuclear oxovanadium(V) complexes, [VO2L]2 (L?=?L1?=?2-[(2-methylaminoethylimino)methyl]phenolate (1); L?=?L2?=?2-[(2-ethylaminoethylimino)methyl]phenolate (2); L?=?L3?=?2-[(2-isopropylaminoethylimino)methyl]phenolate (3)), has been synthesized and characterized by physico-chemical methods and single-crystal X-ray diffraction. The V in each complex is octahedral, with three donors of L and one oxo defining the equatorial plane, and with two oxos occupying the axial positions. The complexes were tested for their urease inhibitory activities. The inhibition rate (%) of 1, 2, and 3 at 100?µmol?L?1 on urease are 67?±?1, 53.5?±?0.9, and 44?±?1. The relationship between structures of the complexes and the urease inhibitory activities indicates that shorter terminal groups of the complexes have stronger activities against urease. Molecular docking study of the complexes with the Helicobacter pylori urease was performed.  相似文献   

17.
Abstract

Artemether; a sesquiterpene lactone is widely used for the treatment of malaria as artemisinin-based combination therapy (ACT). The present work involves the development and validation of sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) method for quantification of artemether (ART) in polymeric nanoparticles. ART was transformed to α, β-unsaturated decalones by pre-column acid treatment to enhance the sensitivity of chromophoric group lacking ART for quantification by HPLC-UV. Waters Spherisorb® 5?µm ODS(C18) column (4.6*250?mm) with gradient elution by mobile phase comprising of ACN and PBS (10?mM; pH 6.0) was used to separate acid-treated ART. The analysis was carried at λmax of 253?nm with 20?min and 20?µL run time and injection volume, respectively. The method was found to be linear in the concentration range of 0.5–10?µg mL?1 with 0.09?µg mL?1 and 0.27?µg mL?1 as LOD and LOQ respectively. Further, the method was also found to be specific for ART in presence of blank polymeric nanoparticles, accurate (% average recovery rate 101.7?±?1.68%), precise (RSD <2%), and robust. The method was successfully used to determine % entrapment efficiency and in vitro release of ART-loaded polymeric nanoparticles with HPLC using a UV-visible detector.  相似文献   

18.
New cadmium(II) complexes with phosphine telluride ligands of the type CdX2(R3PTe)n [X?=?ClO4?, n?=?4: R?=?n-Bu (1), Me2?N (2), C5H10?N (3), C4H8?N (4) or OC4H8?N (5); X?=?Cl, n?=?2: R?=?n-Bu (6), Me2?N (7), C5H10?N (8), C4H8?N (9) or OC4H8?N (10)] have been synthesized and characterized by elemental analyses, IR and multinuclear (31P, 125Te, and 113Cd) NMR spectroscopy. In particular, the solution structures of these complexes were confirmed by 113Cd NMR at low temperature, which displays a quintuplet for each of the perchlorate complexes and a triplet for each of the chloride complexes due to coupling with four and two equivalent phosphorus atoms, respectively, indicating a four-coordinate tetrahedral geometry for the metal center. These multiplet features were further accompanied by one bond Te–Cd couplings, clearly showing that the ligand is coordinated to the metal through tellurium. The results are discussed and compared with those obtained for closely related phosphine chalcogenide analogs.  相似文献   

19.
Binuclear ruthenium(III) complexes [RuX3L]2?·?nH2O (X?=?Cl, L?=?L1, L2, L3; n?=?1, L4 and L5, X?=?Br; L?=?L3), [RuX3L1.5]2?·?nH2O (X?=?Br, L?=?L1; n?=?0, L4; n?=?6 and L5; n?=?10), and [RuX3L2]2 (X?=?Br, L?=?L2) have been isolated by treatment of hydrated RuX3 (X?=?Cl/Br) in acetone with 2-(2′-aminophenylbenzimidazole) (L1), 2-(3′-aminophenylbenzimidazole) (L2), 2-[(3′-N-salicylidinephenyl)benzimidazole] (L3), 2-(3′-pyridylbenzimidazole) (L4), and 2-(4′-pyridylbenzimidazole) (L5) in acetone. The complexes were characterized by elemental analysis, conductivity and magnetic susceptibility measurements, IR, electronic, EPR, and mass spectral studies. The complexes were dimeric; based on analytical and spectral studies, an octahedral geometry was proposed for the complexes. The synthesized complexes were screened against Gram-positive and Gram-negative bacteria and fungi.  相似文献   

20.
A series of binuclear Schiff-base complexes of zinc(II) and mercury(II) containing bidentate ligands (HL) [HL?=?salicylidene-2-methyl-1-aminobenzene (HL1), salicylidene-2-aminopyridine (HL2), and salicylidene-3-nitro-1-aminobenzene (HL3)] with “N” and “O” donors have been synthesized by simple metathetic reactions of anhydrous metal chlorides with sodium salts of Schiff bases (in tetrahydrofuran (THF)/MeOH) in equimolar ratio to produce [(µ-Cl)2M2(L)2?·?xTHF] [where M?=?Zn(II) and Hg(II); L?=?HL1, HL2, and HL3; x?=?0 for (1), (4), (6) and x?=?2 for (2), (3), (5)]. The main emphasis on the complexes [(µ-Cl)2M2(L)2?·?2THF] (2), (3), and (5) is given due to their five-coordinate environment around metal ions. The complexes have been characterized by elemental analyses (M, Cl, C, H, N), melting point, and spectral (FT-IR, 1H-NMR, and 13C-NMR) studies. The structural composition of the complexes has been determined by FAB-MS spectral studies. FAB-MS showed the isotopic molecular ion peak [M+] and fragments supporting the formulation. Powder X-ray diffraction study of 6 is also reported showing the crystallite size (404.5?Å) of the complex.  相似文献   

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