共查询到20条相似文献,搜索用时 15 毫秒
1.
Ewa Bobrowska-Grzesik 《Mikrochimica acta》2001,136(1-2):31-34
Derivative spectrophotometry was applied for the simultaneous determination of amoxycillin and clavulanic acid in pharmaceutical
preparations: “Augmentin” inj. and tablets and “Amoksiklav” drops and tablets, in solutions after hydrolysis with sodium hydroxide.
As the absorption spectra overlap strongly (amoxycillin λmax = 247 nm and 290 nm, clavulanic acid λmax = 258 nm) the first and the second derivative spectrophotometric procedure was elaborated for their determination. Amoxycillin
was determined at λ = 257.9 nm (1-st derivative spectra) or λ = 273 nm (2-nd derivative) while clavulanic acid at λ = 280.3 nm
(1-st derivative) or λ = 285 nm (2-nd derivative spectra). The Beer’s law is obeyed in the range of 0.004–0.04 mg/ml for amoxycillin
and 0.002–0.02 mg/ml for clavulanic acid.
Received December 6, 1999. Revision August 1, 2000. 相似文献
2.
Zora M. Grahovac Snežana S. Mitić Todor G. Pecev Emilija T. Pecev Aleksandra N. Pavlović 《中国化学会会志》2008,55(1):137-142
A new sensitive and simple kinetic method is developed for determination of traces of ascorbic acid based on its activated effect on oxidation of trisodium‐2‐hydroxy‐1‐(4‐sulphonato‐1‐naphthylazo)naphthalene‐6,8‐disulphonato (red artificial color Ponceau 4R) by hydrogen peroxide, in the presence of Cu(II) as catalyst, in borate buffer. The reaction is followed spectrophotometrically by tracing the oxidation product at 478.4 nm within 1 min after addition of H2O2. The optimum reaction conditions are: borate buffer (pH = 11.00), Ponceau 4R (9.6·10?6 mol/L), H2O2 (2·10?2 mol/L), Cu(II) (8·10?7 mol/L) at 22 °C. Following this procedure, ascorbic acid can be determined with a linear calibration graph up to 1.76 ng/mL and a detection limit of 0.28, based on 3S criterion. The relative error ranges between 6.77‐1.66% for the concentration interval of ascorbic acid 1.76‐17.61 ng/mL. The effects of certain foreign ions upon the reaction rate were determined for an assessment of the selectivity of the method. The method was applied for determination of ascorbic acid in pharmaceutical samples, and spectrophotometric method was used like an comparative method. 相似文献
3.
A simple, rapid, selective, sensitive and economical method has been developed for the simultaneous determination of trace
amounts of palladium and nickel in aqueous methanolic medium using 2-(2-thiazolylazo)-5-dimethylam inobenzoic acid as an analytical
reagent by first derivative spectrophotometr y. Palladium is determined by measuring base to peak distance at λ=695.0 nm while
nickel is estimated by zero crossing method in the mixture. The linearity is maintained between 0.12–1.75 μg mL−1 for palladium and 0.07–1.60 μg mL−1 for nickel in the pH range 2.8–7.2 and 3.4–8.8 respectively. Seven replicate determinations of 1.0 μ g mL−1 of palladium and 0.8 μg mL−1 of nickel in a mixture give a mean signal height of 0.391 for Pd and 0.541 for Ni with relative standard deviations of 0.9%
and 1.2%, respectively. The sensitivity of the proposed method is 0.391 (dA/dλ)/(μg mL−1) for palladium and 0.685 (dA/dλ)/(μg mL−1) for nickel. Various parameters have been optimised for the simultaneous determination of palladium and nickel in various
complex samples.
Received March 30, 1999. Revision November 25, 1999. 相似文献
4.
A simple, sensitive and selective kinetic spectrofluorimetric determination of NO2 sampled by the droplet method in the atmosphere was proposed on the basis of the reaction of safranin O with nitrite. By
this reaction, a diazonium salt is formed, which causes a fluorescent reddish-orange dye color of the solution to change into
a non fluorescent blue color. The reaction was monitored fluorimetrically by measuring the decrease in fluorescence intensity
of safranin O at (λex/λem = 536 nm/579 nm) by a fixed-time method. The experimental conditions were optimized. Under the optimum conditions in the
concentration range of 7.5–400 ng/ml, a linear calibration curve (r2 = 0.9978) was obtained with a detection limit of 7.5 ng/ml. The method was applied successful ly to the determination of
nitrite in spiked water and NO2 in the atmosphere, as sampled by a liquid droplet method.
Received August 23, 1999. Revision February 29, 2000. 相似文献
5.
A simple and direct spectrophotometric method has been developed for the determination of cobalt(II) using N,N′-Bis(2-aminobenzoyl)ethylenediamine
(Baben). The method is based on the colour reaction between Baben and cobalt(II) in borax buffer (pH 9.2). The studies are
carried out at 470 nm at which the calculated value of molar absorptivity is found to be 1.102 × 104 L mol−1 cm−1. The system obeys Beer’s law over a wide range of concentration (2–20 μg/ml). The effect of interfering ions has been studied
and the method was applied to the determination of cobalt in water, industrial effluents and in alloys and the results were
highly satisfactory.
Received May 8, 2000. Revision January 30, 2001. 相似文献
6.
Ashraf A. Mohamed 《Monatshefte für Chemie / Chemical Monthly》2001,132(8):919-928
Summary. A new selective, sensitive, and simple kinetic method is developed for the determination of trace amounts of iodide. The
method is based on the catalytic effect of iodide on the reaction of triflupromazine (TFP) with H2O2. The reaction is followed spectrophotometrically by tracing the oxidation product at 498 nm within 1 min after addition of
H2O2. The optimum reaction conditions are TFP (0.4 × 10−3
M), H2SO4 (1.0M), H3PO4 (2.0M), and H2O2 (1.6M) at 30°C. Following this procedure, iodide can be determined with a linear calibration graph up to 4.5 ng ċ cm−3 and a detection limit of 0.04 ng ċ cm−3, based on the 3 Sb criterion. The method can also be applied to the determination of iodate and periodate ions. Determination of as little as
0.2, 1.0, 2.0, and 4.0 ng ċ cm−3 of I−, IO3
-, or IO4
- in aqueous solutions gave an average recovery of 98% with relative standard deviations below 1.6% (n = 5). The method was applied to the determination of iodide in Nile river water and ground waters as well as in various food
samples after alkaline ashing treatment. The method is compared with other catalytic spectrophotometric procedures for iodide
determination.
Received January 19, 2001. Accepted (revised) March 12, 2001 相似文献
7.
Ortega-Algar S Ramos-Martos N Molina-Díaz A 《Analytical and bioanalytical chemistry》2008,391(2):715-719
A single optosensing device based on lanthanide-sensitized luminescence was developed for determination of p-aminobenzoic acid (PABA). The method is based on the formation of a complex between PABA and Tb(III) immobilized on the solid
phase (QAE A-25 resin) placed inside the flow cell. NaCl (1 M) was used as carrier solution and HCl (0.05 M) as eluent. The
sample solutions of PABA (100 μL) containing Tb(III) and buffered at pH = 6.0 were injected into the carrier stream and the
luminescence was measured at λ
ex = 290 nm and λ
em = 546 nm. The method shows a linear range from 0.2 to 6.0 μg mL−1 with an RSD of 1.2% (n = 10) and a sampling frequency of 22 h−1. A remarkable characteristic of the method is its high selectivity which allows it to be satisfactorily applied to the analysis
of PABA in pharmaceutical samples without prior treatment.
Figure Typical emission bands of Tb(III) in a solid-phase PABA–Tb(III) luminescence spectrum 相似文献
8.
Naracham Veedu Sreekumar Ronald Aquin Nazareth Badiadka Narayana Prashant Hegde Busnur Rachotappa Manjunatha 《Mikrochimica acta》2002,140(1-2):63-67
A complexometric method for the determination of mercury in presence of other metal ions based on the selective masking ability
of potassium bromide towards mercury is described. Mercury(II) present in a given sample solution is first complexed with
a known excess of EDTA and the surplus EDTA is titrated against zinc sulfate solution at pH 5–6 using xylenol orange as the
indicator. A known excess of 10% solution of potassium bromide is then added and the EDTA released from Hg-EDTA complex is
titrated against standard zinc sulfate solution. Reproducible and accurate results are obtained for 8 mg to 250 mg of mercury(II)
with a relative error ± 0.28% and standard deviations ≤0.5 mg. The interference of various ions is studied. This method was
applied to the determination of mercury(II) in its alloys.
Received April 18, 2001 Revision October 10, 2001 相似文献
9.
The interactions between proteins and Ponceau 4R (PR) in aqueous solution have been studied by the techniques of resonance light scattering (RLS) spectroscopy, the absorption spectroscopy, zeta potential assay and circular dichroism (CD) spectrum. The dry PR can assemble on the surface of protein via electrostatic and hydrophobic forces to produce an associated compound of protein-PR, this compound can enhance the RLS of protein. Based on this fact, a simple, rapid, and sensitive method has been developed for the determination of proteins at nanogram level by RLS technique with a common spectrofluorimeter. Under optimum conditions, the linear range is 0.10-39.2 μg mL−1 for the determination of both bovine serum albumin (BSA) and human serum albumin (HSA). The detection limits (S/N = 3) are 6.96 ng mL−1 for BSA and 5.71 ng mL−1 for HSA, respectively. There is almost no interference from amino acids, most of the metal ions, and other coexistent substances. The method has been satisfactorily applied to the direct determination of the total protein in human serum. 相似文献
10.
The fluorometric determination of periodate with tetraiodofluorescein has been developed. Under the optimum conditions responses
were linear between 4.0×10−7 ∼ 1.0 × 10−5 mol/L of periodate. The detection limit was 1.0 × 10−7 mol/L corresponding to a signal to noise ratio of 2. The proposed method was applied to the determination of periodate in
artificial fresh water and kelp sample with good results.
Received March 20, 2001 Revision December 19, 2001 相似文献
11.
A rapid flow-injection method with chemiluminescence (CL) detection is described for the determination of glutathione (GSH).
The method is based on the CL reaction of luminol and hydrogen peroxide. GSH can greatly enhance the chemiluminescence intensity
in 0.1 mol/L borax–sodium hydroxide buffer solution (pH = 9.7). The maximum CL intensity was directly proportional to the
concentration of GSH in the range 3.0 × 10−7–2.0 × 10−5 mol/L, and the detection limit was 6.8 × 10−8 mol/L. The relative standard deviation was 3.4% for 5.0 × 10−6 mol/L of GSH (n = 11).
Received October 23, 2001; accepted June 18, 2002 相似文献
12.
In this work, a new ligand, 2,9-bis[N,N-bis(carboxymethyl)-aminomethyl]-1,10-phenanthroline (BBCAP), was synthesized and
used to establish a novel fluorimetric method for the determination of trace amounts of terbium in a binary system. Its luminescence
mechanism was studied. The excitation and emission wavelengths are 284 nm and 547 nm, respectively. Other rare-earth metal
ions in 100-fold excess caused no interference. The fluorescence intensity was a linear function of the concentration of terbium
in the range of 5.0 × 10−10–1.0 × 10−6 mol/L. The detection limit was 2.0 × 10−11 mol/L (n = 12). The standard addition method was used to determine the terbium in a synthetic rare-earth sample with satisfactory
results. This method represents a direct, rapid, selective and sensitive analytical procedure with a widely linear range.
Received November 29, 2001 Revision February 9, 2002 相似文献
13.
Keiichi Satoh Toshio Suzuki Kiyoshi Sawada 《Monatshefte für Chemie / Chemical Monthly》2001,132(10):1145-1155
Summary. The molecular structures of bis-(pyridine base) complexes of cadmium(II) chloride and bromide, where the pyridine base is pyridine ( py), 3-methylpyridine (3-Me-py), 4-methylpyridine (4-Me-py), and 4-ethylpyridine (4-Et-py), were investigated by means of single-crystal X-ray diffraction and Raman spectroscopy. The crystal structures of CdCl2 py
2 (1), CdCl2(3-Me-py)2 (2), and CdCl2(4-Me-py)2 (3) were determined. All crystals are monoclinic; 1: a = 17.784(2), b = 8.666(1), c = 3.8252(7) ?, β = 91.54(1)°, space group: P21/n; 2: a = 11.89(1), b = 14.41(1), c = 3.874(6) ?, β = 92.3(1)°, space group: P21/a; 3: a = 21.091(2), b = 3.8884(5), c = 18.2317(3) ?, β = 113.64(1)°, space group: C2/c. The structures were refined to R/R
w
values (%) of 3.2/5.5, 3.0/5.0, and 3.4/5.1 for 1–3. All cadmium atoms are octahedrally coordinated with the chloride ions forming infinite di-μ-chloro polymeric linear chains
and the nitrogen atoms of the pyridine base in trans configuration. The Cd chains are oriented along the c-axis in 1 and 2 and along the b-axis in 3. The crystal structures indicate the absence of a peculiar interaction between the polymeric chains. The Raman spectra of eight complexes were measured in the range of 550–50 cm−1, and the Raman peaks originating from cadmium-halogen vibrations were assigned. The Raman spectra of 1 and 2 are quite alike in the lattice mode vibration region. The resemblance of the cadmium-halogen vibration peaks indicates the
same halogenide ion bridged octahedral structure for all complexes.
Received March 27, 2001. Accepted (revised) June 19, 2001 相似文献
14.
Three simple and sensitive colorimetric methods (A–C) for the determination of melatonin in bulk samples and in pharmaceutical
formulations are described. They are based on the formation of coloured species by reaction of ninhydrin with the drug (method
A, λmax 397 nm) by oxidation of the indol moiety in melatonin with potassium persulphate (method B, λmax 450 nm) or by reduction of osmium (VIII) (method C, λmax 516 nm). Regression analysis of Beer-Lambert plots showed good correlations in concentration ranges between 0.8–14.2, 70.0–140.0
and 2.0–40.0 μg/mL for methods A, B and C, respectively. The molar absorptivity, Sandell sensitivity and detection limit were
calculated. For more accurate analysis, Ringbom optimum concentration ranges were calculated. The validity of the proposed
methods was tested by analysing pharmaceutical formulations containing melatonin. The relative standard deviations were ≤ 0.95%
with recoveries 99.0–101.33%.
Received October 20, 1999. Revision February 10, 1999. 相似文献
15.
Huang KJ Zhang M Xie WZ Zhang HS Feng YQ Wang H 《Analytical and bioanalytical chemistry》2007,388(4):939-946
A simple, sensitive, selective, and low-cost method is proposed for rapidly determining nitric oxide (NO) in some rat tissues.
Polymer monolith microextraction (PMME) using a poly(methacrylic acid–ethylene glycol dimethacrylate) (MAA-EGDMA) monolithic
column was combined with derivatization of NO using 1,3,5,7-tetramethyl-8-(3′,4′-diaminophenyl)-difluoroboradiaza-s-indacene (TMDABODIPY), and this was used to analyze the derivatives of NO by high-performance liquid chromatography (HPLC)
with fluorescence detection at λ
ex/λ
em = 498/507 nm. The baseline separation of TMDABODIPY and its NO derivative is performed under simple conditions in which a
C18 column is used and eluted with 50 mmol L−1 ethanolamine and methanol. The conditions for the extraction of NO derivatives were optimized. The limit of detection of
NO was 2 × 10−12 mol L−1 (S/N = 3). The linearity range of the method was 9 × 10−11−4.5 × 10−8 mol L−1. The interday and intraday relative standard deviations were less than 5%. The proposed method was successfully applied to
the determination of NO levels in some rat tissue samples including heart, kidney, and liver with recoveries varying from
87.1 to 95.2%. 相似文献
16.
In the presence of carbonate and uranine, the chemiluminescent intensity from the reaction of luminol with hydrogen peroxide
was dramatically enhanced in a basic medium. Based on this fact and coupled with the technique of flow-injection analysis,
a highly sensitive method was developed for the determination of carbonate with a wide linear range. The method provided the
determination of carbonate with a wide linear range of 1.0 × 10−10–5.0 × 10−6 mol L−1 and a low detection limit (S/N = 3) of carbonate of 1.2 × 10−11 mol L−1. The average relative standard deviation for 1.0 × 10−9–9.0 × 10−7 mol L−1 of carbonate was 3.7% (n = 11). Combined with the wet oxidation of potassium persulfate, the method was applied to the simultaneous determination
of total inorganic carbon (TIC) and total organic carbon (TOC) in water. The linear ranges for TIC and TOC were 1.2 × 10−6–6.0 × 10−2 mg L−1 and 0.08–30 mg L−1 carbon, respectively. Recoveries of 97.4–106.4% for TIC and 96.0–98.5% for TOC were obtained by adding 5 or 50 mg L−1 of carbon to the water samples. The relative standard deviations (RSDs) were 2.6–4.8% for TIC and 4.6–6.6% for TOC (n = 5). The mechanism of the chemiluminescent reaction was also explored and a reasonable explanation about chemical energy
transfer from luminol to uranine was proposed.
Figure Chemiluminescence profiles in batch system. 1, Injection of 100 μL of K2CO3 into 1.0 mL luminol-1.0 mL H2O2 solution; 2-3 and 4-5, Injection in sequence of 100 μL of K2CO3 and 100 μL of uranine into 1.0 ml luminol-1.0 mL H2O2 solution; Cluminol = 1.0 × 10−7 mol/L, CH2O2 = 1.0 × 10−5 mol/L, Curanine = 1.0 × 10−5 mol/L, CK2CO3 = 1.0 × 10−7 mol/L except for 4-5 where CK2CO3 = 1.0 × 10−4 mol/L 相似文献
17.
Comparison between Different Hydrolysis Processes of Vine-Trimming Waste to Obtain Hemicellulosic Sugars for Further Lactic Acid Conversion 总被引:1,自引:0,他引:1
Moldes AB Bustos G Torrado A Domínguez JM 《Applied biochemistry and biotechnology》2007,143(3):244-256
Trimming vine shoot samples were treated with water under selected operational conditions (autohydrolysis reaction) to obtain
a liquid phase containing hemicellulose-decomposition products. In a further acid-catalyzed step (posthydrolysis reaction),
xylooligosaccharides were converted into single sugars for the biotechnological production of lactic acid using Lactobacillus
pentosus. A wide range of temperatures, reaction times, and acid concentrations were tested during the autohydrolysis–posthydrolysis
process to investigate their influence on hemicellulose solubilization and reaction products. The maximum concentration of
hemicellulosic sugars was achieved using autohydrolysis at 210 °C followed by posthydrolysis with 1% H2SO4 during 2 h. Data from autohydrolysis–posthydrolysis were compared with the results obtained at the optima conditions assayed
for prehydrolysis (3% H2SO4 at 130 °C during 15 min) based on previous works. Prehydrolysis extracted more hemicellulosic sugars from trimming vine shoots;
however, the protein content in the hydrolysates from autohydrolysis–posthydrolysis was higher. The harsher conditions assayed
during the autohydrolysis process and the higher content of protein after this treatment could induce Maillard reactions decreasing
consequently the concentration of hemicellulosic sugars in the hydrolysates. Therefore, despite the several advantages of
autohydrolysis (less equipment caused by the absence of mineral acid, less generation of neutralized sludges, and low cost
of reagents) the poor results obtained in this work with no detoxified hydrolysates (Q
P = 0.36 g/L h, Q
S = 0.79 g/L h, Y
P/S = 0.45 g/g, Y
P/Sth = 61.5 %) or charcoal-treated hydrolysates (Q
P = 0.76 g/L h, Q
S = 1.47 g/L h, Y
P/S = 0.52 g/g, Y
P/Sth = 71.5 %) suggest that prehydrolysis of trimming vine shoots with diluted H2SO4 is more attractive than autohydrolysis-posthydrolysis for obtaining lactic acid through fermentation of hemicellulosic sugars
with L. pentosus. Besides the higher hemicellulosic sugars concentration achieved when using the prehydrolysis technology, no detoxification
steps are required to produce efficiently lactic acid (Q
P = 1.14 g/L h; Q
S = 1.64 g/L h; Y
P/S = 0.70 g/g; Y
P/Sth = 92.6 %), even when vinification lees are used as nutrients (Q
P = 0.89 g/L h; Q
S = 1.54 g/L h; Y
P/S = 0.58 g/g; Y
P/Sth = 76.1 %). 相似文献
18.
de Jesus Rodrigues Santos W Lima PR Tarley CR Kubota LT 《Analytical and bioanalytical chemistry》2007,389(6):1919-1929
Despite the increasing number of applications of molecularly imprinted polymers (MIP) in analytical chemistry, the synthesis
of polymers with hemin introduced as the catalytic center to mimic the active site of peroxidase remains as a challenge. In
the current work, a new type of molecularly imprinted polymer (MIP) was synthesized with 4-aminophenol (4-APh) as the template
and two monomers: hemin, which acts as the catalytic center, and methacrylic acid (MAA), which is used to build the active
sites. This work shows that MIP successfully mimics peroxidase. For this purpose, a flow injection analysis system coupled
to an amperometric detector was investigated through multivariate analysis. The determination of 4-APh was not affected by
the equimolar presence of structurally similar phenol compounds, including catechol, 4-chloro-3-methylphenol, 2-aminophenol,
guaiachol, chloroguaiachol and 2-cresol, thus highlighting the good performance of the imprinted polymer. Under the optimized
experimental conditions, an analytical curve covering a wide linear response range from 0.8 up to 500 μmol L−1 (r > 0.999) was obtained, and the method gave satisfactory precisions (n = 8), as evaluated via the relative standard deviation (RSD), of 4.1 and 3.2% for solutions of 4-APh of 50 and 500 μmol L−1, respectively. Recoveries of 96–111% from water samples (tap water and river water) spiked with 4-APh were achieved, thus
illustrating the accuracy of the proposed system.
Figure Schematic presentation of the synthesis of the MIP 相似文献
19.
Narachum V. Sreekumar Nellikalaya G. Bhat Badiadka Narayana Ronald A. Nazareth Prashant Hegde Busnur R. Manjunatha 《Mikrochimica acta》2003,141(1-2):29-33
A simple, rapid and accurate complexometric method is proposed for the determination of titanium(IV) where sodium potassium
tartrate or ascorbic acid were used as masking agents. In the presence of diverse metal ions, titanium is first complexed
with excess of EDTA and surplus EDTA is then titrated at pH 5–6 with zinc sulfate, xylenol orange being used as indicator.
An excess of 5% aqueous sodium potassium tartrate is then added to displace the complexed EDTA from the Ti-EDTA complex quantitatively,
which is titrated with zinc sulfate. Also, ascorbic acid may be used as the releasing agent. The methods work well in the
range 1–53 mg of Ti(IV) for sodium potassium tartrate with relative errors ± 0.28% and standard deviations ≤ 0.16 mg. For
ascorbic acid the range is 1.00–30.00 mg of Ti(IV) with relative errors of ± 0.40% and standard deviations of ≤ 0.05 mg
Received October 9, 2001; accepted August 2, 2002 相似文献
20.
Zirconium (IV) was determined spectrophotometrically by reaction with quercetin as primary ligand and oxalate as secondary
ligand. Polyvinylpyrrolidone (PVP) was used as protective colloid to solubilize the formed zirconium quercetin oxalate ternary
complex. The molar absorptivity of the 1:3:1 (zirconium–quercetin–oxalate) complex is 7.31 × 104 L·mol−1 cm−1 at 430 nm with a stability constant of 8.2 × 1020 and its detection limit is 0.16 mg/L. Beer’s law is rectilinear up to 1.46 mg/L of zirconium (IV). The sensitivity index
is 1.25 ng cm−2.
The reaction of aluminium (III) with quercetin in presence of PVP as a surfactant has been studied spectrophotometrically.
The molar absorptivity of the 1:3 (aluminium–quercetin) complex is 8.09 × 104 × L·mol−1·cm−1 at 433 nm, its stability constant is 2.6 × 1013 with sensitivity index of 0.33 ng·cm−2 and its detection limit is 0.08 mg/L. The optimal conditions for the quantitative determination of zirconium and aluminium
were studied. The proposed methods are examined by statistical analysis of the experimental data. The methods are free from
interference of most cations and anions. The proposed methods have been used to determine zirconium and aluminium in industrial
waste water.
Received May 30, 2001; accepted November 2, 2001; published online July 15, 2002 相似文献