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1.
 A simple and sensitive spectrophotometric method is described for the determination of some phenolic antibiotics namely: cefadroxil, amoxicillin and vancomycin. The method is based on the measurement of the orange yellow species produced when the drugs are coupled with diazotized benzocaine in triethylamine medium. The method is applicable over the range of 0.8–12 μg/ml for cefadroxil, 2–16 μg/ml for amoxicillin and 2–18 μg/ml for vancomycin. The formed compounds absorb at 455 nm for both cefadroxil and amoxicillin and at 442 nm for vancomycin. The proposed method has detection limits of 0.018 μg for cefadroxil, 0.0034 μg for amoxicillin and 0.0156 μg for vancomycin. The stoichiometric ratio for the studied compounds was found to be 1:1 and a proposal of the reaction pathway was made. The proposed method was applied for the analysis of the cited drugs in their pharmaceutical preparations. The results are in good agreement with those obtained by the official methods. Received February 7, 2000. Revision June 14, 2000.  相似文献   

2.
Solid-phase extraction (SPE) method for preconcentration and determination of Cd(II), Pb(II), Co(II), Ni(II), and Cu(II) aqueous samples by inductively coupled plasma optical emission spectrometry is described. The preconcentration of analytes is accomplished by retention of their chelates with 1.10-phenanthroline in aqueous solution on a solid phase containing carboxylic acid (COOH) bonded to silica gel in a column. The limits of detection values (defined as “3s” where “s” is standard deviation of the blank determination) are 3.6 μg/L for Cd(II), 17.5 μg/L for Pb(II), 3.1 μg/L for Co(II), 2.1 μg/L for Ni(II), and 4.4 μg/L for Cu(II) and corresponding limit of quantification (6s) values are 7.2, 35, 6.2, 4.2 and 8.8 μg/L, respectively. As a result, a simple method was elaborated for the group concentration and determination of the above mentioned metals in reference material and in samples of plant material. The article is published in the original.  相似文献   

3.
The World Health Organization states that envenomation is responsible for a high number of deaths per year, especially in equatorial areas. The only effective specific treatment is the use of hyperimmune serum (antivenom). In Brazil, Crioula breed horses are used for antivenom production, with great importance in the maintenance of public health programs. A strict biochemical and metabolic control is required to attain specificity in antiserum. Inorganic elements represent only a small fraction of whole blood. Nonetheless, they play important roles in mammalian metabolism, being responsible for controlling enzymatic reactions, respiratory and cardiac functions and ageing. In this work, whole blood samples from Crioula breed horses were analyzed by EDXRF technique. The reference interval values were determined for the elements Na (1955–2013 μg g−1), Mg (51–75 μg g−1), P (523–555 μg g−1), S (1628–1730 μg g−1), Cl (2388–2574 μg g−1), K (1649–1852 μg g−1), Ca (202–213 μg g−1), Cu (4.1–4.5 μg g−1) and Zn (2.4–2.8 μg g−1) and a comparative study with NAA results was outlined. The samples were obtained from Instituto Butantan. Both techniques showed to be appropriate for whole blood sample analyses and offer a new perspective in Veterinary Medicine.  相似文献   

4.
 Two different mass spectrometric methods, negative thermal ionization isotope dilution mass spectrometry (NTI-IDMS) and inductively coupled plasma mass spectrometry (ICP-MS), off-line and on-line coupled with anion exchange chromatography, have been developed for simultaneous bromide and bromate determinations in water samples. The detection limits of these methods are in the range of 0.03–0.09 μg/L using a 50 mL sample.The results are independent of the content of other anions, which could be demonstrated by the analyses of six mineral waters containing chloride and sulfate of up to 160 mg/L and 1500 mg/L, respectively. Bromide has been analyzed by the NTI-IDMS method in the range of 10–500 μg/L and bromate in the range of 1–50 μg/L with relative standard deviations of 0.3–1.2% and 0.4–6%. Quantification for the ICP-MS method was carried out by the standard addition technique, which resulted in relative standard deviations of 5.5% for bromide at the 500 μg/L level and of 13% for bromate at the level of about 3 μg/L. These results are compared with those described in the literature for ion chromatographic (IC) and other methods and those obtained in this work by IC using UV detection, which allows high concentrations of chloride in the bromate fraction. The detection limits of this IC method are 6 μg/L for bromide and 30 μg/L for bromate. NTI-IDMS and ICP-MS therefore fit the recommendations of the European Union (detection limit<2.5 μg/L; precision and accuracy better than 25% at the 10 μg/L level) for methods analyzing the carcinogenic bromate much better than IC and other methods applied up to now. As a definitive but time consuming method, NTI-IDMS is preferably applicable as a calibration technique, whereas ICP-MS, with relatively short analysis times, due to on-line coupling with chromatography, can be used as a sensitive and powerful routine method for trace bromide and bromate species in water samples. Received: 5 July 1996/Accepted: 7 August 1996  相似文献   

5.
 Two different mass spectrometric methods, negative thermal ionization isotope dilution mass spectrometry (NTI-IDMS) and inductively coupled plasma mass spectrometry (ICP-MS), off-line and on-line coupled with anion exchange chromatography, have been developed for simultaneous bromide and bromate determinations in water samples. The detection limits of these methods are in the range of 0.03–0.09 μg/L using a 50 mL sample.The results are independent of the content of other anions, which could be demonstrated by the analyses of six mineral waters containing chloride and sulfate of up to 160 mg/L and 1500 mg/L, respectively. Bromide has been analyzed by the NTI-IDMS method in the range of 10–500 μg/L and bromate in the range of 1–50 μg/L with relative standard deviations of 0.3–1.2% and 0.4–6%. Quantification for the ICP-MS method was carried out by the standard addition technique, which resulted in relative standard deviations of 5.5% for bromide at the 500 μg/L level and of 13% for bromate at the level of about 3 μg/L. These results are compared with those described in the literature for ion chromatographic (IC) and other methods and those obtained in this work by IC using UV detection, which allows high concentrations of chloride in the bromate fraction. The detection limits of this IC method are 6 μg/L for bromide and 30 μg/L for bromate. NTI-IDMS and ICP-MS therefore fit the recommendations of the European Union (detection limit<2.5 μg/L; precision and accuracy better than 25% at the 10 μg/L level) for methods analyzing the carcinogenic bromate much better than IC and other methods applied up to now. As a definitive but time consuming method, NTI-IDMS is preferably applicable as a calibration technique, whereas ICP-MS, with relatively short analysis times, due to on-line coupling with chromatography, can be used as a sensitive and powerful routine method for trace bromide and bromate species in water samples. Received: 5 July 1996/Accepted: 7 August 1996  相似文献   

6.
During the course of a human biomonitoring project (Biebesheim in Hessen, Germany) we elaborated a simple but sensitive method for the determination of tri- (TCP), tetra- (TeCP) and pentachlorophenol (PCP) in human urine. Urine samples, spiked with internal standards, were treated by acid hydrolysis. After a steam bath distillation the distillates were extracted using solid phase extraction. Derivatization of the chlorophenols was not carried out. GC/ECD system was used for detection. Detection limits of the chlorophenols were found in the range of 0.02 μg/L urine (detection limits of the ECD: 0.52 to 2.76 μg/L). By this method mono- and dichlorophenols cannot be detected. We investigated 24h-urine samples of 339 pupils (age 10 to 12 years). The children live either in the surroundings of a hazardous waste incinerator (SVA) in Biebesheim (n = 193), or controls (i.e. regions without waste incinerator) in the non polluted areas of Odenwald (n = 90) and Rheintal (n = 56). Between these three groups we did not find statistically significant differences in chlorophenol concentrations of the urine samples. The 95-percentiles of the analyzed samples are 0.74 μg/L (2,3,4-TCP), 1.24 μg/L (2,3,5-TCP), 0.70 μg/L (2,3,6–TCP), 1.10 μg/L (2,4,5–TCP), 1.74 μg/L (2,4,6–TCP), 2.84 μg/L (3,4,5–TCP), 4.78 μg/L (2,3,4,5-TeCP), 1.86 μg/L (2,3,4,6-TeCP), 2.90 μg/L (2,3,5,6-TeCP) and 4.39 μg/L (PCP). Received: 24 February 1999 / Revised: 3 May 1999 / Accepted: 6 May 1999  相似文献   

7.
During the course of a human biomonitoring project (Biebesheim in Hessen, Germany) we elaborated a simple but sensitive method for the determination of tri- (TCP), tetra- (TeCP) and pentachlorophenol (PCP) in human urine. Urine samples, spiked with internal standards, were treated by acid hydrolysis. After a steam bath distillation the distillates were extracted using solid phase extraction. Derivatization of the chlorophenols was not carried out. GC/ECD system was used for detection. Detection limits of the chlorophenols were found in the range of 0.02 μg/L urine (detection limits of the ECD: 0.52 to 2.76 μg/L). By this method mono- and dichlorophenols cannot be detected. We investigated 24h-urine samples of 339 pupils (age 10 to 12 years). The children live either in the surroundings of a hazardous waste incinerator (SVA) in Biebesheim (n = 193), or controls (i.e. regions without waste incinerator) in the non polluted areas of Odenwald (n = 90) and Rheintal (n = 56). Between these three groups we did not find statistically significant differences in chlorophenol concentrations of the urine samples. The 95-percentiles of the analyzed samples are 0.74 μg/L (2,3,4-TCP), 1.24 μg/L (2,3,5-TCP), 0.70 μg/L (2,3,6–TCP), 1.10 μg/L (2,4,5–TCP), 1.74 μg/L (2,4,6–TCP), 2.84 μg/L (3,4,5–TCP), 4.78 μg/L (2,3,4,5-TeCP), 1.86 μg/L (2,3,4,6-TeCP), 2.90 μg/L (2,3,5,6-TeCP) and 4.39 μg/L (PCP). Received: 24 February 1999 / Revised: 3 May 1999 / Accepted: 6 May 1999  相似文献   

8.
 A reversed-phase HPLC-method for the separation of mixtures of collectors for the flotation of heavy metal minerals is described. It is based on a Nucleosil 5C18 column, isocratic elution and UV-detection at 238 nm. The mobile phase is methanol-water-5% phosphoric acid (40:60:4, v/v). The method is applied to the determination of six collectors in aqueous solutions from flotation processes. The relative standard deviations are 1.6–3.2% in the concentration range 2–10 mg/L. The detection limits are 1 μg/L for 8-hydroxyquinoline, dimethylglyoxime and salicylic acid, 2 μg/L for salicylhydroxamic acid and 5 μg/L for benzenetriazol and salicylaldoxime, respectively. Received: 19 April 1996/Revised: 14 August 1996/Accepted: 23 August 1996  相似文献   

9.
Summary l-Phenylalanine was immobilized on nylon membranes with two pore diameters (0.45 μm and 1 μm), by activation with 1,4-butanediol diglycidyl ether, and the effect of pore size on the affinity adsorption of γ-globulin studied by batch and kinetic methods. Experiment shows that adsorption on both affinity membranes obeys the Freundlich model. The accessible pore volume for adsorption of proteins on the membrane with 0.45 μm diameter pores is less than for that with 1 μm diameter pores. The adsorption capacity of affinity membranes with 1 μm diameter pores is 2.5-fold that of membranes with 0.45 μm diameter pores. Feed-rate has a larger effect on affinity adsorption on the membrane with 0.45 μm diameter pores than on that with 1 μm diameter pores. Small pores on the affinity membrane do not cause broadening of the elution peak. It is concluded that affinity interaction and separation occur mainly in the large pores, and small pore size does not favor improvement of adsorption capacity. γ-Globulin 85.1% pure can be obtained in one step from human plasma by use of the affinity membrane with 0.45 μm diameter pores.  相似文献   

10.
An analytical method for detecting and quantifying cefotaxime in plasma and several tissues is described. The method was developed and validated using plasma and tissues of rats. The samples were analyzed by reversed phase liquid chromatography (HPLC) with UV detection (254 nm). Calibration graphs showed a linear correlation (r > 0.999) over the concentration ranges of 0.5–200 μg/mL and 1.25–25 μg/g for plasma and tissues, respectively. The recovery of cefotaxime from plasma standards prepared at the concentrations of 25 μg/mL and 100 μg/mL was 98.5 ± 3.5% and 101.8 ± 2.2%, respectively. The recovery of cefotaxime from tissue standards of liver, fat and muscle, prepared at the concentration of 10 μg/g was: 89.8 ± 1.2% (liver), 103.9 ± 6.5% (fat) and 97.8 ± 2.1% (muscle). The detection (LOD) and quantitation (LOQ) limits for plasma samples were established at 0.11 μg/mL and 0.49 μg/mL, respectively. The values of these limits for tissues samples were approximately 2.5 times higher: 0.3 μg/g (LOD) and 1.25 μg/g (LOQ). For plasma samples, the deviation of the observed concentration from the nominal concentration was less than 5% and the coefficient of variation for within-day and between-day assays was less than 6% and 12%, respectively. The method was used in a pharmacokinetic study of cefotaxime in the rat and the mean values of the pharmacokinetic parameters are given. Received: 25 May 1998 / Revised: 27 July 1998 / Accepted: 1 August 1998  相似文献   

11.
A sequential injection analysis (SIA) system is described for the determination of phenoxybenzamine hydrochloride and metoclopramide using spectrophotometer as detector. The method is based on the detection of an unstable red intermediate compound resulting from the reaction of phenoxybenzamine hydrochloride or metoclopramide with the diazotizating product of p-phenylenediamine with sodium nitrite in hydrochloric acid medium. The sampling frequency is 69 h−1 and 75 h−1 for phenoxybenzamine hydrochloride and metoclopramide, respectively. The linear range is 10–400 μg/mL for phenoxybenzamine hydrochloride with a detection limit of 0.081 μg/mL and 20–250 μg/mL for metoclopramide with a detection limit of 0.034 μg/mL. The RSD is 1.01 and 0.45% for phenoxybenzamine hydrochloride and metoclopramide, respectively. The proposed methods were used to determine phenoxybenzamine hydrochloride and metoclopramide in pharmaceuticals. The results are compared with those obtained by pharmacopoeia method. The article is published in the original.  相似文献   

12.
The present work reports on the synthesis, characterization and performance of a new iron(III)-containing ionic liquid [(C4H9)2-bim][FeCl4] (Fe-IL, bim = benzimidazolium) as an electrocatalyst for nitrite and bromate reduction. The melting point of Fe-IL is 70 °C. Thermal behavior of the Fe-IL was studied by differential scanning calorimetry and thermalgravimetry. The value of magnetic moment and its temperature dependence were measured. A conductive carbon paste electrode (Fe-IL/CPE) comprised of Fe-IL and carbon powder was fabricated by the direct mixing method. The Fe-IL has double functions—a binder and an electrocatalyst. The electrochemical behavior and electrocatalysis of Fe-IL/CPE have been studied by cyclic voltammetry. The Fe-IL/CPE shows excellent electrocatalytic activities toward nitrite and bromate reduction. The detection limit and the sensitivity are 0.01 μM and 100.58 μA μM−1 for nitrite, and 0.01 μM and 83.11 μA μM−1 for bromate detection, respectively. This work demonstrates that the Fe-IL may become a new kind of functional material in constructing chemicals and biosensors.  相似文献   

13.
A novel electrochemical sensor is prepared by electropolymerization with p-aminobenzenesulfonic acid (p-ABSA) film and dropping graphene oxide on the surface of electrode. The results indicated that GO-poly(p-ABSA) nanofilms displayed enhanced current responses to dopamine and serotonin. In the range of 0.3–20 μmol dm−3 and 0.6–20 μmol dm−3, the dopamine and serotonin concentration are linearly related to current intensity, and the detection limit is 0.09 μmol dm−3 and 0.2 μmol dm−3 (S/N = 3), respectively. By adding dopamine and serotonin standards, the electrochemical sensor is applied in serum sample. The results show that the GO-poly(p-ABSA) films represent well-modified materials for use in the biosensors.  相似文献   

14.
A novel method is proposed for the extraction-thermal lens quantification of cobalt with Nitroso-R-Salt based on the distribution of the colored complex in a two-phase aqueous system on the basis of poly-ethylene glycol (PEG) and an ammonium sulfate solution followed by its thermal lens detection in the extract. The limit of detection is 0.3 μM (20 ng/mL); the lower limit of the analytical range is 0.7 μM (40 ng/mL); the relative standard deviation for the concentrations 1–50 μM makes 1–3% (n = 6, P = 0.95). In the determination of cobalt by spectrophotometry under the same conditions, the detection limit is 10 μM (0.6 μg/mL) and the lower limit of the analytical range is 40 μM (2.5 μg/mL). The precision of thermal lens measurements in PEG solutions is higher in comparison to that in aqueous ones because of the weaker interference of convection in aqueous solutions of PEG.  相似文献   

15.
A poly(methyl methacrylate) microfluidic chip was used to perform a two-dimensional (2-D) separation of a complex protein mixture in short development times. The separation was performed by combining sodium dodecyl sulfate micro-capillary gel electrophoresis (SDS μ-CGE) with microemulsion electrokinetic chromatography (μ-MEEKC), which were used for the first and second dimensions, respectively. Fluorescently labeled Escherichia coli cytosolic proteins were profiled by this 2-D approach with the results compared to a similar 2-D separation using SDS μ-CGE × μ-MEKC (micelle electrokinetic chromatography). The relatively short column lengths (effective length = 10 mm) for both dimensions were used to achieve separations requiring only 220 s of development time. High spot production rates (131 ± 11 spots min−1) and reasonable peak capacities (481 ± 18) were generated despite the fact that short columns were used. In addition, the use of μ-MEEKC in the second dimension was found to produce higher peak capacities compared to μ-MEKC (481 ± 18 for μ-MEEKC and 332 ± 17 for μ-MEKC) due to the higher plate numbers associated with μ-MEEKC.  相似文献   

16.
A growing body of evidence indicated that the G protein coupled receptors exist as homo- or hetero-dimers in the living cell. The heterodimerization between μ and δ opioid receptors has attracted researchers’ particular interests, it is reported to display novel pharmacological and signalling regulation properties. In this study, we construct the full-length 3D-model of μ and δ opioid receptors using the homology modelling method. Threading program was used to predict the possible templates for the N- and C-terminus domains. Then, a 30 ns molecular dynamics simulations was performed with each receptor embedded in an explicit membrane-water environment to refine and explore the conformational space. Based on the structures extracted from the molecular dynamics, the likely interface of μ–δ heterodimer was investigated through the analysis of protein–protein docking, cluster, shape complementary and interaction energy. The computational modelling works revealed that the most likely interface of heterodimer was formed between the transmembrane1,7 (TM1,7) domains of μ receptor and the TM(4,5) domains of δ receptor, with emphasis on μ-TM1 and δ-TM4, the next likely interface was μ(TM6,7)-δ(TM4,5), with emphasis on μ-TM6 and δ-TM4. Our results were consistent with previous reports. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.  相似文献   

17.
This paper describes optimization and validation of a method for sulfadiazine determination in milk samples based on sulfadiazine derivatization with fluorescamine followed by excitation–emission (fluorescence) measurement. For both the optimization and the validation, a comparison between zero-order and first-order signals has been made, showing the advantages of using first-order signals. In the optimization the effects of the temperature of the derivatization reaction, the amount of fluorescamine and the derivatization time on the instrumental signal (maximum intensity or the net analyte signal) are studied by a factorial experimental design, with the optimal values of these factors which give the highest signal being 22 °C for the reaction temperature, 50 μl fluorescamine and 20 min of derivatization time. The validation of the method under the optimal experimental conditions shows that the analytical method is fit-for-purpose, with values of the capability of detection (CCβ) of 4.3 μg l−1 at a sulfadiazine concentration of zero and with probabilities of a false positive and a false negative of 5%. Around the permitted limit (established for the sulfonamides at 100 μg l−1), CCβ is 112 μg l−1. The precision, as the intermediate reproducibility, was established as 1.2 and 3.3 μg l−1 around 0 and 100 μg l−1, respectively. In the application to milk samples spiked with sulfadiazine a mean recovery of around 90% was obtained with a standard deviation of about 8% (14 samples of different concentrations).  相似文献   

18.
A diffusion junction between two paired gold electrodes is created in a bipotentiostatic electro-deposition process. Gold metal is deposited simultaneously on two adjacent disc electrodes (100 μm diameter, approximately 125 μm separation) until short-circuit conditions trigger the end point of the electro-deposition. Symmetric gold junctions with typically 5 μm average inter-electrode gap size, 140 μm gap length, and approximately 18 μm junction depth are obtained. These paired gold electrodes are employed in generator–collector mode to give well-defined steady-state feedback currents even for extremely low concentrations of analyte (sub-μM) and without any contributions from capacitive charging. Four redox systems are investigated spanning a wide range of diffusion coefficients: (1) the one-electron oxidation of iodide to iodine, (2) the two-electron oxidation of hydroquinone to benzoquinone, (3) the two-electron reduction of alizarin red S, and (4) the one-electron oxidation of the redox protein cytochrome c. Consistent results for these redox systems suggest that (1) the junction zone between the two electrodes is dominating the behaviour of the electrode in particular for the slower diffusing systems and (2) the paired gold electrode junction can be calibrated and employed for electroanalysis at very low concentrations and for a wider range of analytically relevant redox systems. Dedicated to Professor Keith B. Oldham, on the occasion of his 80th birthday  相似文献   

19.
This study evaluated the effects of alloxan on the kinetics properties of the δ-aminolevulinate dehydratase (δ-ALA-D) using mouse liver homogenates. δ-ALA-D is an important sulfhydryl enzyme that catalyses the second step in heme biosynthesis and is commonly diminished in experimental and human diabetes. Despite the known effects of alloxan in models of experimental diabetes, there are no data in the literature demonstrating the effects of alloxan on the kinetics properties of the δ-ALA-D. The results showed that alloxan (1.25–20 μM) caused a concentration-dependent inhibition of hepatic δ-ALA-D activity. The inhibition constant (K i ) for alloxan-induced inhibition on δ-ALA-D was 3.64 μM. The alloxan (5 μM) caused a decrease in V max (65.8%) and in K m (53.1%), which is suggestive of an uncompetitive inhibition of enzyme. In addition, dithiothreitol (700 and 1,000 μM) completely prevented the δ-ALA-D activity inhibition induced by 10 and 20 μM alloxan. Similar protection was obtained in the presence of 2,000 μM glutathione. Therefore, this work showed that the inhibition of hepatic δ-ALA-D activity can be obtained in vitro at low micromolar levels of alloxan, and can also be prevented by reducing agents. Moreover, these results may help to understand the abnormalities in heme pathway found in models of experimental diabetes in vivo.  相似文献   

20.
Glassy carbon electrode modified with electrodeposited nickel oxide nanoparticles (NiOxNPs) was used as electrocatalyst for oxidation of omeprazole and pentoperazole in alkaline solution. The modified electrode exhibited efficient electrocatalytic activity for the oxidation of omeprazole and pentoperazole with relatively high sensitivity, excellent stability, and long lifetime. Hydrodynamic amperometric method is used for determination of selected analytes. Under optimized condition, the linear concentration range, detection limit, and sensitivity of modified electrode toward omeprazole detection are 4.5–120 μM, 0.4 μM (at signal to noise 3), and 40.1 nA μM−1 cm−2, respectively. For pantoperazole, hydrodynamic amperometric determination yielded calibration curve with linear range of 2.5–180 μM, detection limit of 0.2 μM, and sensitivity of 39.2 nA μM−1 cm−2, respectively. The proposed method was successfully applied to pentoperazole and omeprazole determination in drug samples.  相似文献   

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