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1.
A novel rapid and sensitive analytical method, enhanced chemiluminescence with flow-injection sampling, is described for determination
of ciprofloxacin. The method is based on the chemiluminescence reaction of the potassium permanganate–sodium thiosulfate–ciprofloxacin
system. An enhanced chemiluminescence reaction was developed, and optimum conditions for CL emission were investigated. The
chemiluminescence intensity was linearly dependent on ciprofloxacin concentration in the range 1.0×10−8–1.0×10−5 g mL−1. The detection limit was 4×10−9 g mL−1. The relative standard deviation was 1.8% for eleven measurements of 2.0×10−7 g mL−1 ciprofloxacin standard solution. The new method enables simple, sensitive, and rapid determination of ciprofloxacin and has
been successfully used for determination of ciprofloxacin in biological fluids and in ciprofloxacin hydrochloride tablet and
injection. 相似文献
2.
A fluorimetric procedure for the determination of sulfamethoxazole using flow injection analysis is proposed. A two channel system is optimized for the fluorescent reaction with o-phthaldialdehyde and β-mercaptoethanol. The detection limit is 0.007 μg/ml. No fluorescence is generated by the metabolite N-acetylated sulfamethoxazole. The method is applied to the determination of sulfamethoxazole in pharmaceuticals, urine and bovine serum samples without matrix interference problems. 相似文献
3.
Flow-injection chemiluminescence determination of epinephrine in pharmaceutical preparations using raw apple juice as enzyme source 总被引:3,自引:0,他引:3
Raw apple juice exhibits the activity of polyphenol oxidase which can be employed for the determination of mono-, di- and polyhydric phenols. The chemiluminescence detection in the two-channel manifold was used to develop the new procedure for determination of epinephrine. Epinephrine can be determined by this method in pharmaceutical preparations in concentration ranges 1.0–10.0 and 10.0–25.0 mg l−1, with a detection limit of 0.2 mg l−1. Good selectivity against typical antioxidants and other coexisting substances was achieved. Relatively slow loss of the enzyme activity was observed during 1 week. The proposed method is very simple. Fresh juice solution from one apple can be prepared in 10 min and used for at least 8 h with excellent precision. Consumption of luminol solution was 0.15 ml min−1. The throughput was 20 samples per hour. 相似文献
4.
A novel chemiluminescence method for the determination of levofloxacin is presented, which is based on the inhibitory effect
of levofloxacin on the chemiluminescence reaction between luminol and myoglobin in a flow-injection system. The decrement
of chemiluminescence intensity is linear with the logarithm of levofloxacin concentration over the range from 0.07 to 100.0
ng/mL (r
2 = 0.9994), with the detection limit of 0.02 ng/mL (3σ). At a flow rate of 2.0 mL/min, a complete analytical process could
be performed within 0.5 min, including sampling and washing, with a relative standard deviation of less than 3.0% (n = 5). The proposed procedure was applied successfully to the determination of levofloxacin in pharmaceutical preparations,
human urine and serum without any pretreatment procedure. 相似文献
5.
A flow-injection configuration is proposed for the individual determination of cysteine and cystine and for the mixtures of both analytes. The procedure is based on the inhibitory effect of cysteine on the oxidation of thiamine to thiochrome by mercury(II). Linear calibration graphs were obtained between 1.0 x 10(-5) and 1.0 x 10(-4)M, with a sampling rate of 22 samples/hr and relative standard deviation of 1.14%. The inclusion of a selecting valve in the configuration, to pump water or hydroxylamine, allows the successive determination of these two analytes. The applicability of the method to the determination of cysteine and cystine in pharmaceutical preparations was demonstrated by investigating the effect of potential interferences and by the analysis of commercial preparations. 相似文献
6.
A flow-injection configuration for the fluorimetric determination of trimeprazine and trifluoperazine is proposed. The procedure is based on oxidation of the drugs by cerium(IV). The fluorescence of cerium(III) formed in the oxidation of trimeprazine or trifluoperazine is monitored. Lineal calibration graphs were obtained between 2 x 10(-7) and 1 x 10(-5)M for both trimeprazine and trifluoperazine with a sampling rate of 60 samples/hr. The relative standard deviations were over the ranges 0.78-1.16 and 0.84-0.97% for trimeprazine and trifluoperazine respectively. The applicability of the method to determination of trimeprazine and trifluoperazine was demonstrated by investigating the effect of potential interferences and by analysis of commercial pharmaceutical preparations. 相似文献
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9.
A simple and highly sensitive spectrofluorometric method was developed for the determination of some 1,4-dihydropyridine compounds
namely, nicardipine, nifedipine and isradipine in pharmaceutical preparations and biological fluids. The method is based on
the reduction of nicardipine, nifedipine and isradipine with Zn/HCl and measuring the fluorescence intensity obtained (λem/λex) at 460/364, 450/393 and 446/360 nm, respectively. The factors affecting the development of the fluorophore and its stability
were studied and optimized. The effect of some surfactants such as β-cyclodextrin (βCD), carboxymethylcelullose (CMC), sodium
dodecyl sulphate (SDS) and triton X-100, on the fluorescence intensity was studied. The fluorescence intensity-concentration
plots of nicardipine, nifedipine and isradipine were rectilinear over the ranges 0.4–6.0, 0.2–4.0 and 0.1–9.0 μg ml−1 with detection limits of 0.0028, 0.017 and 0.016 μg ml−1, respectively. The proposed method was successfully applied to commercial tablets containing the compounds; the percentage
recovery agreed well with those obtained using the official methods. The method was further extended to the in vitro determination
of the compounds in spiked human plasma and urine samples. A proposal of the reduction reaction pathway was postulated.
相似文献
10.
A simple, sensitive and accurate spectrophotometric method has been described for the assay of diphenhydramine hydrochloride (DPH) in raw material and in biological samples. The method is based on extraction of DPH into dichloromethane as ion-pair complexes with patent blue (PB), eriochrome black T (EBT), methyl orange (MO) and bromocresol purple (BCP) in acidic medium. The coloured species exhibited absorption maxima at 632, 514, 428 and 414 nm for PB, EBT, MO and BCP, with molar absorptivity values of 1.32 × 105, 2.36 × 104, 3.68 × 104 and 3.07 × 104 l mol?1 cm?1, respectively. The reaction conditions were optimized to obtain the maximum colour intensity. Beer’s law was obeyed with a good correlation coefficient (0.9982–0.9993) in the concentration ranges 0.5–3, 2.0–16, 2.0–10 and 1.0–10 μg ml?1 for PB, EBT, MO and BCP methods, respectively. The composition ratio of the ion-association complexes was found to be 1:1 in all cases as established by Job’s method. The conditional stability constant (Kf) and the free energy changes (ΔG°) were determined for all complexes formed. The proposed method was successfully applied for the determination of DPH in tablets and human urine with good accuracy and precision. Statistical comparison of the results with those obtained by the official method showed good agreement and indicated no significant difference in accuracy and precision. 相似文献
11.
Clobutinol (Cb) ion-selective plastic-membrane electrodes based on ion associates of clobutinolium phosphotungstate (Cb-PTA),
clobutinolium phosphomolybdate (Cb-PMA), or a mixture of both Cb-PTA and PMA were prepared. The electrodes were fully characterized
in terms of membrane composition, life span, pH, and temperature. The electrodes were applied to the potentiometric determination
of clobutinol in pure form and pharmaceutical preparations under batch and flow-injection conditions. Also, conductimetric
titrations were applied to the assay of clobutinol in its pure form and pharmaceutical preparations. The selectivity of the
electrodes towards a large number of inorganic cations, amino acids, and sugars was tested. The solubility product of ion-associates
and the formation constant of the precipitation reactions leading to the ion-associate formation were determined conductimetrically.
The text was submitted by the authors in English. 相似文献
12.
A simple flow injection chemiluminescence (FI-CL) method was proposed for the determination of nitrofurazone. Strong CL signal was generated during the reaction of nitrofurazone with H2O2 and N-bromosuccinimide (NBS) in alkaline condition. The CL signal was proportional to the nitrofurazone concentration in the range 1.0 × 10−7 to 1.0 × 10−5 g mL−1. The detection limit was 2 × 10−8 g mL−1 nitrofurazone and the relative standard deviation was less than 4% (6.0 × 10−6 g mL−1 nitrofurazone, n = 11). The proposed method was successfully applied to the determination of nitrofurazone in compound furacillin nasal drops, human plasma and urine samples. The CL reaction mechanism was also discussed briefly. Singlet oxygen generated in the reaction between H2O2 and NBS was suggested to be participated in the CL reaction. 相似文献
13.
The performance characteristic of sensitive screen-printed (SPE) and carbon paste (CPE) electrodes was investigated for the determination of diphenhydramine hydrochloride (DPH) drug in pure, pharmaceutical preparations and biological fluids. Different experimental conditions namely types of materials used to prepare the working electrode (plasticizer), titrant, pH, temperature and life time were studied. Under these conditions, the SPE shows the best performance than CPE with respect to total potential change and potential break at the end point. The SPE and CPE exhibit suitable response to DPH in a concentration range of 1.0.10− 2 to 1.0.10− 6 mol/L with a limit of detection 9.70.10− 7 and 9.80.10− 7 mol/L, respectively. The slope of the system was 55.2 ± 1.0 and 54.7 ± 1.0 mV/decade over pH range 3.0–8.0 and 3–7 for SPE and CPE, respectively. Selectivity coefficients for DPH relative to a numbers of potential interfering substances were investigated. The SPE and CPE show a fast response time of 10 and 16 s and were used over a period of 2 months with a good reproducibility. The sensors were applied successfully to determine DPH in pharmaceutical preparations and biological fluids. The results are compared with the official method. 相似文献
14.
The construction and general performance characteristics of a novel potentiometric PVC membrane sensor based on pethidine-phosphomolybdate as electroactive material for the determination of pethidine are described. This sensor exhibits fast, stable and near-Nernstain response 55.24 +/- 0.1, over the concentration range 1.10(-2)-1.10(-5)M for pethidine-phosphomolybdate over pH 2-7. No interferences are caused by many organic, inorganic cations, alkaloids and amino acids. The sensor proved useful for determining pethidine in pure forms, pharmaceutical injections and monitoring the content uniformity assay of ampoules. The designed sensor also show good accuracy for the determination of pethidine in biological fluids. 相似文献
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16.
Francisco W. P. Ribeiro Thisiania R. V. Soares Sameque do N. Oliveira Luisa C. Melo Janete E. Soares Helena Becker Djenaine De Souza Pedro de Lima-Neto Adriana N. Correia 《Journal of Analytical Chemistry》2014,69(1):62-71
The electrochemical behaviour and analytical detection procedure for nimesulide (NIM) and ofloxacin (OFX) and their assay in commercial formulations were evaluated using square-wave voltammetry (SWV) combined with a hanging mercury drop electrode (HMDE). All experimental and voltammetric conditions were previously optimized to obtain the best analytical signal in terms of intensities and profile of the reduction peaks. For NIM, the peak currents were related to the one-electron reduction of a nitro group to a stable radical anion, which is followed by a one-electron transfer and a protonation step with a consequent formation of a nitrosoanion. The voltammetric results indicated that the mechanism of OFX involved the transfer of two electrons and two protons in a totally irreversible reduction related to the conversion of a ketone group to an alcohol group. Analytical parameters such as linearity range, equations of the analytical curves, correlation coefficients, detection and quantification limits, recovery efficiency, and relative standard deviation for repeatability and reproducibility experiments were compared to similar results obtained by the use of UV-Vis spectrophotometry, and the results showed that the voltammetric procedure using HMDE is suitable to determine pharmaceutical compounds in complex samples. The applicability of the proposed procedure was tested on pharmaceutical formulations of NIM and OFX by observing the stability, specificity, recovery and precision of the procedure in tablets, oral solution and ophthalmic solution. 相似文献
17.
Differential pulse polarographic determination of ofloxacin in pharmaceuticals and biological fluids
A sensitive method is described for the determination of ofloxacin in its pure form, dosage forms and biological fluids. The proposed method depends upon the polarographic activity of ofloxacin in Britton Robinson buffers, whereby a well-defined cathodic wave is produced over the pH range 4.1-10.3. The wave was characterized as being irreversible, diffusion-controlled with limited adsorption properties. The current-concentration relationship was found to be rectilinear over the range 5x10(-5)-5x10(-4) M and 1x10(-5)-5x10(-4) M using the DC(t) and DPP modes respectively, with a minimum detectability (S/N=3) of 3x10(-7) M. The proposed method was successfully applied to the determination of ofloxacin in tablets and biological fluids. The results obtained were found to be in agreement with those obtained by a reference method. 相似文献
18.
Khoo Lay See Abdalla A. Elbashir Bahruddin Saad Abdussalam Salhin Mohamed Ali Hassan Y. Aboul‐Enein 《Biomedical chromatography : BMC》2009,23(12):1283-1290
A simple, rapid and validated capillary electrophoretic method has been developed for the separation and determination of ofloxacin and ornidazole in pharmaceutical formulations with detection at 230 nm. Optimal conditions for the quantitative separations were investigated. Analysis times shorter than 4 min were obtained using a background electrolyte solution consisting of 25 mmol/L phosphoric acid adjusted with 1 m Tris buffer to pH 8.5, with hydrodynamic injection of 5 s and 20 kV separation voltage. The validation criteria for accuracy, precision, linearity and limits of detection and quantitation were examined and discussed. An excellent linearity was obtained in concentration range 25–250 µg/mL. The detection limits for ofloxacin and ornidazole were 1.03 ± 0.11 and 1.80 ± 0.06 µg/mL, respectively. The proposed method has been applied for the analysis of ofloxacin and ornidazole both individually and in a combined dosage tablet formulation. The proposed validated method showed recoveries between 96.16 and 105.23% of the nominal contents. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
19.
A modification of the Trautz-Schorigin reaction into a flow-injection analysis configuration is described. Different approaches were used at the optimization of chemiluminescence determination of formaldehyde in water based on the reaction of formaldehyde, gallic acid and hydrogen peroxide in an alkaline solution. Detection system with a 218 μl chemiluminescence cell was optimized by both a one-variable-at-a-time method, and a modified simplex method. A calibration graph is linear in the concentration range 4 × 10−8 to 1 × 10−5 M HCHO. The detection limit of formaldehyde for a signal-to-noise ratio of 3 is 4 × 10−8 M. The relative standard deviations for 15 repeated measurements of 1 × 10−6 and 5 × 10−6 mol l−1 HCHO are 4.32 and 3.33%, respectively. The analysis time is 1.5 min. The method was applied to the determination of formaldehyde in urban rainwater. A comparison of results found by proposed method with those obtained by fluorimetric reference method provided a good agreement. 相似文献