Determination of enalapril maleate and atenolol in their pharmaceutical products and in biological fluids by flow‐injection chemiluminescence

A chemiluminescent method using flow injection (FI) was investigated for rapid and sensitive determination of enalapril maleate and atenolol, which are used in the treatment of hypertension. The method is based on the sensitizing effect of these drugs on the Ce(IV)–sulfite reaction. The different experimental parameters affecting the chemiluminescence (CL) intensity were carefully studied and incorporated into the procedure. The method permitted the determination of 0.01–3.0 µg mL^?1 of enalapril maleate in bulk form with correlation coefficient r = 0.99993, lower limit of detection (LOD) 0.0025 µg mL^?1 (S/N = 2) and lower limit of quantitation (LOQ) 0.01 µg mL^?1. The linearity range of atenolol in bulk form was 0.01–2.0 µg mL^?1 (r = 0.99989) with LOD of 0.0003 µg mL^?1 (S/N = 2) and LOQ of 0.01 µg mL^?1. In biological fluids the linearity range of enalapril maleate was 0.1–2.0 µg mL^?1 in both urine and serum, and for atenolol the linearity range was 0.1–1.0 µg mL^?1 in both urine and serum. The method was also applied to the determination of the drugs in their pharmaceutical preparations. Copyright © 2009 John Wiley & Sons, Ltd.     

Effects of desiccation and rewetting on the release and decomposition of dissolved organic carbon from benthic macroalgae

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Resonance light scattering study on the interaction between quinidine sulfate and congo red and its analytical application

The interaction between quinidine sulfate (QDS) and congo red (CR) was studied using resonance light scattering (RLS) technique, ultraviolet–visual spectrophotometry and fluorimetry. In weak acidic medium, QDS reacts with CR to form a supermolecular complex which results in the enhanced RLS intensity. Some important interacting parameters, such as the solution acidity and CR concentration, salt effect and addition order of the reagents, were investigated and optimized. Under the optimum conditions, it was found that the enhanced RLS intensity was in proportion to the concentration of QDS in the range 0.2–8.4 µg mL^?1. The corresponding detection limit was 12.0 ng mL^?1. The results showed that this new method enabled simple, sensitive and rapid determination of QDS and was used for the determination of QDS in urine and simulated huamn serum samples. Copyright © 2009 John Wiley & Sons, Ltd.     

Using blood plasma cortisol concentration and fish behaviour to determine temperature avoidance in the estuarine‐dependent fish species Rhabdosargus holubi (Steindachner, 1881) (Sparidae)

In order to test the hypothesis that a combination of blood cortisol measurements and behavioural observations can be used to estimate the avoidance temperature of the estuarine‐dependent Cape stumpnose, Rhabdosargus holubi (Steindachner, 1881) (Sparidae), fish were kept at increasing water temperatures at a rate of 3°C d^?1 over 7 days. Plasma cortisol concentrations were significantly influenced by the interaction of time and treatment (F = 10.9, P < 0.01) with cortisol concentrations in fish kept at increasing temperature averaging 293 ng ml^?1 on day 7. This was 5.4 times higher than the average value for control fish (29 ng ml^?1). For the first 6 days, average cortisol concentration of control fish was 25.7 ± 5.0 ng ml^?1, while values for fish from the temperature treatment ranged from 8.3 to 176.6 ng ng ml^?1. These values combined with behaviour observations suggest that cortisol concentration and behavioural changes may be used to detect both a low and an acute stress response.     

Micelle‐enhanced spectrofluorimetric method for quantification of entacapone in tablets and human plasma

In this paper, a simple and highly sensitive spectrofluorimetric method was developed and validated for the determination of entacapone (ETC). The proposed method is based on forming a highly fluorescent product through the reduction of ETC with Zn/HCl. The produced fluorophore exhibits strong fluorescence at λ_em 345 nm after excitation at λ_ex 240 nm. The use of fluorescence enhancers such as Tween‐80 and carboxy methyl cellulose (CMC) greatly enhanced the fluorescence of the produced fluorophore by 150% and 200%, respectively. Calibration curves showed good linear regression (r2 > 0.9998) within test ranges of 0.05–2.0 and 0.02–1.80 μg mL^?1 with lower detection limits of 1.27 × 10^?2 and 4.8 × 10^?3 μg mL^?1 and lower quantification limits of 4.21 × 10^?2 and 1.61 × 10^?2 μg mL^?1 upon using Tween‐80 and or CMC, respectively. The method was successfully applied to the analysis of ETC in its pharmaceutical formulations (either alone or in presence of other co‐formulated drugs). The results were in good agreement with those obtained using the official method. The methods were further extended to determine the drug in human plasma samples, and to study the pharmacokinetics of ETC. The paper is the first report on the spectrofluorimetric determination of entacapone.     

Simultaneous chiral separation of tramadol and methadone in tablets,human urine,and plasma by capillary electrophoresis using maltodextrin as the chiral selector

The stereoselective analysis and separation of racemic drugs play an important role in pharmaceutical industry to eliminate the unwanted isomer and find the right therapeutic control for the patient. Present study suggests a maltodextrin‐modified capillary electrophoresis method for a single‐run chiral separation of two closely similar opiate pain relief drugs: tramadol (TRA) and methadone (MET). The best separation method possible for the both enantiomers was achieved on an uncoated fused‐silica capillary at 25°C using 100 mM phosphate buffer (pH 8.0) containing 20% (w v^?1) maltodextrin with dextrose equivalent of 4–7 and an applied voltage of 16 kV. Under optimal conditions, the baseline resolution of TRA and MET enantiomers was obtained in less than 12 minutes. The relative standard deviations (n = 3) of 20 μg mL^?1 TRA and MET were 2.28% and 3.77%, respectively. The detection limits were found to be 2 μg mL^?1 for TRA and 1.5 μg mL^?1 for MET. This method was successfully applied to the measurement of drugs concentration in their tablets, urine, and plasma samples.     

A highly sensitive fluorescent probe for tiopronin based on the cleavage of 2, 4‐dinitrobenzenesulfonate

A highly sensitive fluorogenic probe for tiopronin was proposed. 2,4‐Dinitrobenzenesulfonyl‐fluorescein (I) is an almost nonfluorescent compound. Upon mixing with tiopronin in aqueous solution, the 2,4‐dinitrobenzenesulfonyl group of I was efficiently removed and its parent dye fluorescein was released, hence leading to dramatic increases in both fluorescence and absorbance of the reaction mixture. Under optimal conditions, the fluorescence increase is linear with tiopronin concentration in the range 5.0–600 ng mL^?1, with a detection limit of 1.5 ng mL^?1 (3σ). The proposed method has been successfully applied to tiopronin determination in pharmaceutical preparations and in spiked human urine samples. Copyright © 2009 John Wiley & Sons, Ltd.     

Investigation of the binding of AuNPs–6‐mercaptopurine and the sensitive detection of 6‐mercaptopurine using resonance Rayleigh light scattering

A highly sensitive method for the detection of 6‐mercaptopurine (MP) by resonance Rayleigh light scattering (RLS) method was developed. Gold nanoparticles (AuNPs) were synthesized by a modified seed method and characterized using transmission electron microscopy (TEM). AuNPs were bound to MP via covalent bonding to form the MP–AuNPs complex, which increased the RLS intensity of MP at 347 nm (increased by 65.7%). Under optimum conditions, the magnitude of the enhanced RLS intensity for MP–AuNPs was proportional to MP concentration in the range 0.0681–1.702 μg mL^?1. The linear regression equation was represented as follows: ΔI _RLS = 9.31 + 82.42c (r  = 0.9948). The limit of detection (LOD, 3σ) was 3.32 ng mL^?1. The system was applied successfully to detect MP in pharmaceuticals. MP recoveries were 99.9–101.7% with a relative standard deviation (RSD) (n  = 5) of 0.59–0.77% for three synthetic samples, and 97.5–110.0% with an RSD of 0.98–2.10% (n =  5) for tablet samples.     

Nonlinear response of stream ecosystem structure to low‐level phosphorus enrichment

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Highly efficient antibacterial diblock copolypeptides based on lysine and phenylalanine

A series of amphiphilic diblock copolypeptides (K₃₀‐b ‐F₁₅, K₃₀‐b ‐F₃₀, and K₃₀‐b ‐F₄₅) were synthesized via N ‐carboxy‐α‐amino‐anhydride ring‐opening polymerization. The copolypeptides had excellent antibacterial efficacy to both Gram positive (S. aureus ) and Gram negative (E. coli ) bacteria. The minimum inhibitory concentrations (MICs) against E. coli and S. aureus are 8 μg mL^?1 and 2 μg mL^?1, respectively, lower than most natural and artificial antimicrobial peptides (AMPs). The morphological changes of the bacteria treated with diblock copolypeptides were investigated by transmission electron microscopy; the results proved that the diblock copolypeptides had a similar antibacterial pore‐forming mechanism to natural cationic peptides. This was confirmed by laser scanning confocal microscope images. CCK‐8 results and the MICs showed that the diblock copolypeptides have high selectivity to bacteria, which suggested that the diblock copolypeptides could be excellent candidates to replace traditional antibiotics in future.     

Soil carbon and belowground carbon balance of a short‐rotation coppice: assessments from three different approaches

Uncertainty in soil carbon (C) fluxes across different land‐use transitions is an issue that needs to be addressed for the further deployment of perennial bioenergy crops. A large‐scale short‐rotation coppice (SRC) site with poplar (Populus) and willow (Salix) was established to examine the land‐use transitions of arable and pasture to bioenergy. Soil C pools, output fluxes of soil CO₂, CH₄, dissolved organic carbon (DOC) and volatile organic compounds, as well as input fluxes from litter fall and from roots, were measured over a 4‐year period, along with environmental parameters. Three approaches were used to estimate changes in the soil C. The largest C pool in the soil was the soil organic carbon (SOC) pool and increased after four years of SRC from 10.9 to 13.9 kg C m^?2. The belowground woody biomass (coarse roots) represented the second largest C pool, followed by the fine roots (Fr). The annual leaf fall represented the largest C input to the soil, followed by weeds and Fr. After the first harvest, we observed a very large C input into the soil from high Fr mortality. The weed inputs decreased as trees grew older and bigger. Soil respiration averaged 568.9 g C m^?2 yr^?1. Leaching of DOC increased over the three years from 7.9 to 14.5 g C m^?2. The pool‐based approach indicated an increase of 3360 g C m^?2 in the SOC pool over the 4‐year period, which was high when compared with the ?27 g C m^?2 estimated by the flux‐based approach and the ?956 g C m^?2 of the combined eddy‐covariance + biometric approach. High uncertainties were associated to the pool‐based approach. Our results suggest using the C flux approach for the assessment of the short‐/medium‐term SOC balance at our site, while SOC pool changes can only be used for long‐term C balance assessments.     

Effect of dietary L‐malic acid supplementation on growth,feed utilization and digestive function of juvenile GIFT tilapia Oreochromis niloticus (Linnaeus, 1758)

Two feeding trials (FTs) were conducted in 2013 and 2014, respectively, to determine the optimal L‐malic acid (LMA) level for juvenile GIFT (Genetically Improved Farmed Tilapia) Oreochromis niloticus. Except for the LMA level, the FT1 and FT2 had a similar diet formulation. In FT1, LMA was included at 0 (basal diet), 1, 4, 8, 16 and 32 g kg^?1, respectively. After 20 weeks, daily weight gain and feed conversion ratio were improved but not differentiated with 1–8 g kg^?1 LMA. Further increasing the LMA supply initially decreased the feed intake (16 g kg^?1), and then decreased both feed intake and feed utilization (32 g kg^?1), thus impairing the fish growth. FT2 was subsequently conducted with a smaller LMA range (0, 0.5, 1, 2, 4 and 8 g kg^?1, respectively) but was unfortunately terminated at the end of 8 weeks because 20% of the fish were badly injured during weighing. Unexpectedly, growth and feed utilization were still improved but not differentiated with 0.5–8 g kg^?1 LMA. In FT2, beneficial effects of LMA inclusion on the digestive function (pepsin, foregut amylase and foregut lipase), the activities of serum lysozyme and hepatic superoxide dismutase, and liver lipid peroxidation (malondialdehyde concentration) were found. Taking the results of FT1 and FT2 together, it could be concluded that dietary LMA supplementation at low concentrations (0.5–8 g kg^?1) could improve growth and feed utilization, but excess LMA (≥16 g kg^?1) might compromise feed intake and/or feed utilization, thus impairing fish growth. To reduce feed costs in commercial practice, 0.5 g kg^?1 LMA is recommended in the feed of juvenile GIFT tilapia based on the results of this study.     

Limnology and trophic status of glacial lakes in the tropical Andes (Cajas National Park,Ecuador)

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Determination of nucleic acid by [tetra‐(3‐methoxy‐4‐hydroxyphenyl)]–Tb3+ porphyrin as the fluorescence spectral probe in bis(2‐ethylhexyl)sulfosuccinate sodium salt micelle system

A new system for the determination of nucleic acid by rare earth metallic porphyrin of [tetra‐(3‐methoxy‐4‐hydroxyphenyl)]–Tb³⁺ [T(3‐MO‐4HP)–Tb³⁺] porphyrin as fluorescence spectral probe has been developed in this paper. Nucleic acid can enhance the fluorescence intensity of the T(3‐MO‐4HP)–Tb³⁺ porphyrin in the presence of bis(2‐ethylhexyl)sulfosuccinate sodium salt(AOT) micelle. In pH 8.00 Tris–HCl buffer solution, under optimum conditions, the enhanced fluorescence intensity is in proportion to the concentration of nucleic acids in the range of 0.05–3.00 µg mL^?1 for calf thymus DNA (ct DNA) and 0.03–4.80 µg mL^?1 for fish sperm DNA(fs DNA). Their detection limits are 0.03 and 0.01 µg mL^?1, respectively. In addition, the binding interaction mechanism between T(3‐MO‐4HP)–Tb³⁺ porphyrin and ct DNA is also investigated by resonance scattering and fluorescence spectra. The maximum binding number is calculated by molar ratio method. The new system can be used for the determination of nucleic acid in pig liver, yielding satisfactory results. Copyright © 2009 John Wiley & Sons, Ltd.     

Production rate estimation of mycosporine‐like amino acids in two Arctic melt ponds by stable isotope probing with NAH13CO3

The net carbon uptake rate and net production rate of mycosporine‐like amino acids (MAAs) were measured in phytoplankton from 2 different melt ponds (MPs; closed and open type pond) in the western Arctic Ocean using a ¹³C stable isotope tracer technique. The Research Vessel Araon visited ice‐covered western‐central basins situated at 82°N and 173°E in the summer of 2012, when Arctic sea ice declined to a record minimum. The average net carbon uptake rate of the phytoplankton in polycarbonate (PC) bottles in the closed MP was 3.24 mg C · m^?3 · h^?1 (SD = ±1.12 mg C · m^?3 · h^?1), while that in the open MP was 1.3 mg C · m^?3 · h^?1 (SD = ±0.05 mg C · m^?3 · h^?1). The net production rate of total MAAs in incubated PC bottles was highest (1.44 (SD = ±0.24) ng C · L^?1 · h^?1) in the open MP and lowest (0.05 (SD = ±0.003) ng C · L^?1 · h^?1) in the closed MP. The net production rate of shinorine and palythine in incubated PC bottles at the open MP presented significantly high values 0.76 (SD = ±0.12) ng C · L^?1 · h^?1and 0.53 (SD = ±0.06) ng C · L^?1 · h^?1. Our results showed that high net production rate of MAAs in the open MP was enhanced by a combination of osmotic and UVR stress and that in situ net production rates of individual MAA can be determined using ¹³C tracer in MPs in Arctic sea ice.     

Virus dynamics in a large epishelf lake (Beaver Lake,Antarctica)

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Pharmacokinetics of oxytetracycline in yellow catfish [Pelteobagrus fulvidraco (Richardson, 1846)] with a single and multiple‐dose oral administration

A pharmacokinetic study of oxytetracycline (OTC) following a single (100 mg kg^?1) or a multi‐dose (100 mg kg^?1 for 5 days) oral administration was carried out in yellow catfish, Pelteobagrus fulvidraco. After oral administration at 25°C, a one‐compartment model was developed. The absorption half‐life (t_1/2(ka)) was 3.92, 1.44, 2.75, and 3.34 h in plasma, muscle, liver, and kidney after the single dose, and 0.35, 0.22, 0.42, 0.32 h after the multi‐dose, respectively. The order of peak concentration (C_max) was liver > kidney > plasma > muscle, at 3.48 μg g^?1, 2.90 μg g^?1, 1.46 μg ml^?1, and 1.39 μg g^?1 after the single dose, and 14.02 μg g^?1, 8.51 μg g^?1, 4.17 μg ml^?1, and 3.84 μg g^?1 after the multi‐dose, respectively. The elimination half‐lives (t_1/2(ke)) of OTC in plasma, muscle, liver, and kidney were calculated to be 7.64, 26.29, 19.08, and 10.61 h after the single dose, and 47.54, 70.99, 49.87, and 47.73 h after the multi‐dose, respectively. The results suggest that OTC was absorbed faster after the multi‐dose than after the single dose, suggesting that OTC could be more efficacious after the multi‐dose and more effective in the control bacterial diseases in aquaculture, with the side effects of longer withdrawal periods.     

Microbially enhanced dissolution of HgS in an acid mine drainage system in the California Coast Range

Mercury sulfides (cinnabar and metacinnabar) are the main ores of Hg and are relatively stable under oxic conditions (K_sp = 10^?54 and 10^?52, respectively). However, until now their stability in the presence of micro‐organisms inhabiting acid mine drainage (AMD) systems was unknown. We tested the effects of the AMD microbial community from the inoperative Hg mine at New Idria, CA, present in sediments of an AMD settling pond adjacent to the main waste pile and in a microbial biofilm on the surface of this pond, on the solubility of crystalline HgS. A 16S rRNA gene clone library revealed that the AMD microbial community was dominated by Fe‐oxidizing (orders Ferritrophicales and Gallionellas) and S‐oxidizing bacteria (Thiomonas sp.), with smaller amounts (≤6%) being comprised of the orders Xanthomondales and Rhodospirillales. Though the order Ferritrophicales dominate the 16S rRNA clones (>60%), qPCR results of the microbial community indicate that the Thiomonas sp. represents ~55% of the total micro‐organisms in the top 1 cm of the AMD microbial community. Although supersaturated with respect to cinnabar and metacinnabar, microcosms inoculated with the AMD microbial community were capable of releasing significantly more Hg into solution compared to inactivated or abiotic controls. Four different Hg‐containing materials were tested for bacterially enhanced HgS dissolution: pure cinnabar, pure metacinnabar, mine tailings, and calcine material (processed ore). In the microcosm with metacinnabar, the presence of the AMD microbial community resulted in an increase of dissolved Hg concentrations up to 500 μg L^‐1 during the first 30 days of incubation. In abiotic control microcosms, dissolved Hg concentrations did not increase above 100 ng L^?1. When Hg concentrations were below 50 μg L^‐1, the Fe‐oxidizing bacteria in the AMD microbial community were still capable of oxidizing Fe(II) to Fe(III) in the AMD solution, whereas concentrations above 50 μg L^?1 resulted in inhibition of microbial iron oxidation. Our experiments show that the AMD microbial community contributes to the dissolution of mercury sulfide minerals. These findings have major implications for risk assessment and future management of inoperative Hg mines worldwide.     

Sensitive determination of protein based on the fluorescence enhancement effect of terbium (III)–epinephrine–protein–sodium dodecylsulfate system

It was found that the fluorescence of Tb³⁺–epinephrine (E) complex can be enhanced by both bovine serum albumin (BSA) and sodium dodecylsulfate (SDS), and stabilized by ascorbic acid (AA). It is considered that the fluorescence enhancement of the Tb³⁺–E–BSA–AA–SDS system originates not only from the hydrophobic microenvironment provided by BSA–SDS, but also from the energy transfer from BSA to Tb³⁺ in this system. Therefore, a new fluorescence method for the determination of protein concentrations as low as 1.3 × 10^?9 g mL^?1 BSA is established using Tb³⁺–epinephrine complex as probe. The method has been applied for the determination of BSA and human serum albumin in actual samples, and the results obtained are satisfactory. Compared with other fluorescence methods, this method is simpler and more sensitive for the determination of protein. The mechanism of the fluorescence enhancement of the system is studied in detail. Copyright © 2009 John Wiley & Sons, Ltd.     

Effects of the Cry1Ac toxin of Bacillus thuringiensis on Microplitis mediator, a parasitoid of the cotton bollworm, Helicoverpa armigera

Interactions between the cotton bollworm, Helicoverpa armigera (Hübner) (Lepidoptera: Noctuidae), its larval parasitoid Microplitis mediator (Haliday) (Hymenoptera: Braconidae), and the Cry1Ac toxin of Bacillus thuringiensis Berliner were evaluated under laboratory conditions. The growth of H. armigera larvae was delayed and its pupal rate and pupal weight decreased when they were fed on a diet containing Cry1Ac toxin. Due to the lowered growth rate of the host larvae, the time available for parasitization of H. armigera by M. mediator increased when the host larvae were reared on a diet containing Cry1Ac toxin at concentrations of 0.5, 1, 2, and 4 µg g^?1. The longevity of female and male parasitoids was not significantly affected when newly emerging wasps fed on honey solutions containing three different concentrations of Cry1Ac toxin (125, 250, and 500 µg ml^?1). When female parasitoids were fed on honey solutions containing Cry1Ac, their offsprings’ egg and larval development period, pupal weight, length of pupation, adult weight, and adult longevity did not change significantly in most of the treatments compared with controls. When the female parasitoids parasitized host larvae that had been fed on a diet containing 0.5, 1, 2, 4, and 8 µg g^?1 Cry1Ac toxin, their offsprings’ eggs and larvae were significantly delayed. Their pupal weight, adult weight, and adult longevity were also significantly less than controls.