Spectrophotometric determination of some antiamoebic and anthelmintic drugs with metol and chromium(VI)

A sensitive spectrophotometric method is reported for the determination of tinidazole (TZ), metronidazole (MZ), benzoyl metronidazole (BMZ) or niclosamide (NS) either in pure form or in formulations. This method is based on reduction with zinc dust and hydrochloric acid followed by reaction with metol and potassium dichromate at pH 3.0 +/- 0.2 to give a coloured product having maximum absorbance at 720 nm (for TZ, MZ and BMZ) or 530 nm (for NS).     

Electrochemical reduction and voltammetric determination of metronidazole at a nanomaterial thin film coated glassy carbon electrode

Simple and sensitive electrochemical method for the determination of metronidazole, based on a nanostructured film coated glassy carbon electrode (GCE), is described. Multi-walled carbon nanotubes (MWNT) was dispersed into water in the presence of a hydrophobic surfactant to give very stable and homogeneous MWNT suspension, and a MWNT-film coated GCE was achieved via evaporating solvent. Metronidazole yields a well-defined reduction peak whose potential is −0.71 V at the MWNT-film coated GCE in pH 9.0 Britton-Robinson buffer. Compared with bare GCE, the MWNT-film modified GCE significantly enhances the reduction peak current of metronidazole. All the experimental parameters were optimized for the determination of metronidazole. The detection limit is 6×10⁻⁹ mol/l at 2 min accumulation. This method has been successfully used to determine metronidazole in the drugs. Furthermore, results obtained by the proposed method have been compared with spectrophotometric method.     

Studies on reactivity of benzoyl and benzoylperoxy radicals produced by laser flash photolysis of dibenzoyldiazene in aerated solutions

Photolysis of dibenzoyldiazene gives benzoyl radicals. In aerated solutions, the benzoyl radicals react with oxygen to yield benzoylperoxy radicals. Spin trapping studies indicate that 5,5′dimethyl-1-pyrroline N-oxide reacts with the benzoylperoxy radicals to produce the adduct which exhibits ESR parameters, A_N = 13.8 G and A_Hβ = 10.1 G. Laser photolysis studies reveal that the rate constants for the reaction between the benzoyl radical and oxygen are ca. 4 × 10⁹ M^-1 s^-1 in toluene, acetone, and ethyl acetate. The benzoylperoxy radicals undergo one-electron oxidation of tetramethyl-p-phenylenediamine, TMPD, to give an ion pair. The ion pair has an absorption spectrum similar to that of the TMPD cation radical. The formation of the ion pair is detected by monitoring the absorbance change at 600 nm after laser pulsing. From the kinetic studies for the formation of the ion pair in the presence of olefins, the bimolecular rate constants for reactions between several olefins and the benzoylperoxy radical are determined. The electrophilic addition of the benzoylperoxy radicals to olefins is discussed in comparison with the addition reactions of thiyl radicals to olefins. The detection and determination of the dipole moments of both the benzoylperoxy radicals and the ion pair are carried out with the use of the time-resolved microwave dielectric absorption technique. The distance between the positive and negative ions in the ion pair is estimated as 0.20 nm.     

用紫外-可见分光光度计测定油样中沥青质含量

介绍了一种用分光光度法测定油品中的沥青质含量的方法。通过测定样品悬浮液在７５０ｎｍ、８００ｎｍ下的吸光度而获得样品中正庚烷沥青质含量,阐述了方法的测量原理,讨论了取样量范围、沥青地方法的影响。结果表明,该法可应用于各种油品（如原油、重质馏分油、渣油和沥青等）的分析,具有简单、快速的优点,相对标准偏差小于３％。     

Novel Metronidazole Membrane Sensor Based on a 2,6‐(p‐N,N‐Dimethylaminophenyl)‐4‐Phenylthiopyrylium Perchlorate

A novel PVC‐based membrane sensor based on 2,6‐(p‐N,N‐dimethylaminophenyl)‐4‐phenylthiopyrylium perchlorate (DAPP) is described. The electrode exhibits a sub‐Nernstian response to 1‐(beta‐hydroxyethyl)‐2‐methyl‐5‐nitroimidazole (metronidazol) over a relatively wide concentration range (1.0 × 10^?1 to 1.0 × 10^?5 M) with a detection limit of 8.0 × 10^?6 M. The best performance was obtained with the membrane containing 30% poly (vinyl chloride), 50% dibutyl phthalate, 7% DAPP and 13% oleic acid. It has a fast response time (< 30 s) and can be used for at least four weeks without any major deviation. The proposed sensor revealed very good selectivity for metronidazole over a wide variety of common cations, anions and amino acids and could be used in the pH range of 6.0–7.5. It was successfully used for direct determination of metronidazole in an oral synthetic antiprotozoal as an antibacterial agent, in metronidazole tablets, and metronidazole injections and metronidazole gels.     

Drugs of abuse in a non-conventional sample; detection of methamphetamine and its main metabolite, amphetamine in abusers' clothes by HPLC with UV and fluorescence detection.

In this paper, we report the detection of methamphetamine and its major metabolite, amphetamine, in garments belong to known-abusers. These compounds were extracted from the textile using a mixture of chloroform:propan-2-ol (3:1, v/v), derivatized with 4-(4,5-diphenyl-1H-imidazol-2-yl) benzoyl chloride and separated using a reversed-phase high-performance liquid chromatography. The derivatives were detected by measuring either fluorescence at 440 nm or absorbance at 330 nm. By using 1-methyl-3-phenyl propylamine as an internal standard, calibration curves of spiked textile samples were linear over a wide range with correlation coefficients of 0.997 or better. Detection limits at a signal-to-noise ratio of 3 were less than or equal to 37.3 and 0.4 pg on column for the high-performance liquid chromatography-ultraviolet and -fluorescence detection methods, respectively. Intra- and inter-day variations at high and low concentrations (n > or = 3) were < or =12.7%. The developed methods were successfully applied to the determination of methamphetamine and amphetamine in clothes samples belong to abusers.     

Simultaneous Determination of Micro Bromide and Iodide by Kinetic Spectrophotometric Method

ABSTRACT

ABSTRACTA new kinetic spectrophotometric method for the simultaneous determination of concentrations of micro bromide and iodide has been proposed. It is based on their catalytic effects on the reaction of m-cresol purple oxidized by potassium periodate in hydrochloride acid medium. The reaction rate was monitored by measuring the decrease in absorbance at 528nm and the increase in absorbance at 455nm. The total difference in absorbance of the sum of bromide and iodide is identical with determination of bromide was carried out after Cr(VI) oxidized I? to I₂, and I₂ was removed by extraction with CCI₄, and the amount of iodide was measured by subtracting the absorbance change of bromide from the total absorbance change in the presence of bromine and iodide. The optimum conditions influencing the reaction rate were studied. The linear range of determination is 0～4.0μg/ml for Br? and 0～3.0 μg/ml for I?. The detection limits are 0.032μg/ml for Br? and 0.059 μ/ml for I?. The method was successfully applied to the determination of micro amounts of bromide and iodide in food and life samples.     

硫酸铜-酒石酸钾钠-头孢克洛体系分光光度法测定头孢克洛

根据头孢克洛在碱性酒石酸铜溶液中能形成棕黄色配合物,建立了分光光度法测定头孢克洛的新方法。头孢克洛的浓度在32.5~175mg/L范围内与吸光度呈良好的线性关系,线性相关系数为0.994,方法的检出限为0.24mg/L,回收率为96.2%~101.0%。该法可用于胶囊和干混悬剂中头孢克洛含量的测定。     

A fluorimetric kinetic method for the determination of organophosphorus and organocarbonyl compounds

A direct reaction rate method is proposed for the rapid, sensitive determination of organophosphorus and organocarbonyl compounds, based on a fluorimetric SCHOENEMANN reaction. From 0.02 to 100 μg/ml of benzoyl chloride, benzoyl bromide, phthalic anhydride, diisopropyl phosphorofluoridate, parathion, methyl parathion, diethyl chlorophosphate and dimethyl chlorothiophosphate can be determined with an accuracy and precision of about 1.5%.     

Highly sensitive kinetic spectrophotometric method for tramadol trace level detection and process optimization using response surface methodology

Tramadol is a centrally acting analgesic‐anodyne agent of high oral bioavailability. The tramadol contains a weakly absorbing chromophore in its molecule and it was determined by kinetic spectrophotometric method in pharmaceutical, urine, and blood plasma. Response surface methodology and the central composite design was applied to study the influence of maximum sensitivity, reagents concentration, temperature, and time on the UV–Vis spectrophotometry analysis of tramadol. Analysis of variance showed a high coefficient of determination (R²) value for responses, confirming adjustment of the models with experimental data. The change in absorbance was followed spectrophotometrically at 478 nm. Under optimum experimental conditions, calibration curve was linear over the range 0.45–100.0 μg/L of tramadol. The limit of detection was 0.12 μg/L of tramadol. The developed method was successfully applied for the determination of tramadol in real samples.     

BPR光度法检测Fenton反应产生的羟自由基

提出检测Fenton反应产生羟自由基的新方法。羟自由基与溴邻苯三酚红（BPR）发生氧化反应后,溴邻苯三酚红的颜色发生变化,用紫外－分光光度计测定其△A560值的变化,可间接测定羟自由基的产生量。试验结果表明,△A560与溴邻苯三酚红、FeSO4及H2O2呈量效关系,随反应时间延长,△A560依幂函数规律上升。同时发现甘露醇、苯甲酸清除羟自由基作用呈明显的量效关系。方法稳定性好、操作简便、测定快速,可作为一种简便的筛选抗氧化剂的方法。     

A simplified measurement procedure and portable electronic photometer for disposable sensors based on ionophore-chromoionophore chemistry for potassium determination

A field-portable photometer for potassium determination with disposable sensors has been developed. It can be applied to routine water and beverage analysis. The disposable sensor is based on ionophore-chromoionophore chemistry. A colour change in the sensing film is detected by measuring the transmitted intensity with a solid state photodetector. Optical excitation at 660 nm is emitted by a light-emitting diode (LED). Negative feedback for LED bias and thermal correction were included to improve system stability. Additionally, a measurement procedure is presented, characterized and validated for in situ photometer use and real-time results. This simplified procedure is based on prior preparation of the disposable sensor in its acidic form and on the use of an absorbance ratio as analytical parameter. The only requirement for analysis is prior equilibration with a buffered sample solution for 3 min and absorbance measurement before and after equilibration. Good sensitivity in the concentration range 5 μM to 100 mM and very good repetitively and stability were achieved that are comparable to those obtained with bulkier analytical instrumentation. Given the compact size, low weight, rapid response and low energy requirement of the electronic photometer developed here, this measurement system is suitable for potassium determination in the field.     

Chemiluminescence method for determination of benzoyl peroxide in solution

The chemiluminescence reaction of benzoyl peroxide with triethylamine is used to quantify benzoyl peroxide. The method is rapid with a detection limit for benzoyl peroxide in chloroform of 0.07 μg ml^?1 and a relative standard deviation of 4% at 1 μg ml^?1. The technique is applied to the determination of benzoyl peroxide in pharmaceutical preparations.     

高效液相法测定面粉中的过氧化苯甲酰

 报道了测定面粉中过氧化苯甲酰含量的一种改进方法。面粉直接以石油醚萃取 ,采用Shim PackVP ODS柱 (0 46cmi d × 1 5cm ,5μm～ 6μm) ,以乙腈 体积分数为 0 3 %的磷酸水溶液 (体积比为 4∶1 )为流动相 ,流速1 0mL/min ,检测波长 2 36nm。在此条件下 ,过氧化苯甲酰和苯甲酸的质量浓度分别和其峰面积呈良好的线性关系 ,过氧化苯甲酰的线性范围为 0 0 0 2 g/L～ 0 0 1 2 g/L(r =0 9995) ,最小检测量为 0 0 0 5g/kg;苯甲酸的线性范围为 0 0 0 2g/L～ 0 0 1 2g/L (r =0 9993) ,最小检测量为 0 0 1g/kg。     

Spectrophotometric Quantitation of Fluoxetine Hydrochloride Using Benzoyl Peroxide and Potassium Iodide

 Fluoxetine hydrochloride reacts with benzoyl peroxide and potassium iodide, after heating for 1 min at 30 °C, to give a blue colour having maximum absorbance at 570 nm. The reaction is selective for fluoxetine with 0.01 mg/mL as visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer’s law from 0.1 mg/10 mL to 2.0 mg/10 mL of fluoxetine and the relative standard deviation is 0.68%. The qualitative assessment of tolerable amounts of other drugs is also studied. Received September 21, 1998. Revision September 10, 1999.     

Kinetic‐Spectrophotometric Determination of Metronidazole Benzoate in Surfactant Medium

A kinetic method for the accurate and sensitive determination of metronidazole benzoate (MB) has been described. The method is based on the oxidation of MB with KMnO₄ in alkaline medium in the presence of sodium dodecyl sulphate (SDS). At a fixed time of 10 min, the formed magnate ion is spectrophotometrically measured at 610 nm. The determination of MB by the fixed‐concentration and rate constant method is feasible with the calibration equation obtained, but the fixed‐time method proves to be more applicable. The proposed method was successfully used for the quantitative determination of MB in suspended oral syrup after the separation of MB with a simple separation method. Beer's law was obeyed from 0.55 mgL^?1 to 33 mgL^?1 and the RSD% value for syrup was 3.44. The results obtained agreed with those obtained by the BP method.     

过氧化苯甲酰的测定与应用研究

本文提出了一种以丙酮为溶剂,柠檬酸为催化剂和掩蔽剂的间接磺量法以测定过氧化苯甲酰。该方法简便易行,重现性好,准确度高,测定结果令人满意。     

Spectrophotometric determination of urea in dermatologic formulations and cosmetics

A rapid, relatively sensitive, and low-cost method for the determination of water-soluble urea content in dermatological therapy products and cosmetics is proposed using a new spectrophotometric assay with water as the only extraction solvent. Spectrophotometric methods involve addition of a known excess of bromate to urea in an acid medium, followed by the determination of residual bromine and chlorine reacting with methyl orange and measurement of absorbance at 505 nm. The absorbance increases linearly with urea concentration (r = 0.9998). The systems obey Beer's law for 6 - 90 microg ml(-1). The calculated apparent molar absorbance values are found to be 4.537 x 10(3) dm(3) mol(-1) cm(-1) and the Sandell's sensitivity is 0.013 microg cm(-2). The variables affecting the rate of the reaction were investigated. The relative standard deviation for five-replication determination of 60 microg ml(-1) urea was 2.1% and the detection limit of the method is 0.34 ng ml(-1).     

Voltammetry and determination of metronidazole at a carbon fiber microdisk electrode

The electrochemistry of metronidazole, 1-(hydroxyethyl)-2-methyl-5-nitroimidazole, was investigated at a carbon fiber microdisk electrode in pH 9 Britton Robinson buffer. Under these conditions, the reduction of metronidazole is controlled by both mass transport to the microdisk and adsorption with an equilibrium constant of 4 × 10³ mol⁻¹ dm³ and a saturation coverage of 0.88 × 10⁻⁸ mol cm⁻². The adsorption and accumulation of metronidazole on the surface of the carbon fiber allows its determination at low concentrations by square wave adsorptive stripping voltammetry. A detection limit for metronidazole of 5 × 10⁻⁷ mol dm⁻³ and a R.S.D. of 3.7% at 1 × 10⁻⁶ mol dm⁻³ (n = 4) were obtained with a two electrode system with no stirring during the accumulation step. Based on this method, a simple procedure for the determination of metronidazole in urine is described which requires no pre-treatment of the sample before analysis.     

IR spectral determination of mica in multicomponent systems

A procedure for the determination of mica (muscovite) in ores and concentrates by IR spectrometry is developed. It is shown that the change in the absorbance of the muscovite OH group band at 3620 cm^?1 allows a calibration plot to be constructed for the determination of 1–90% muscovite.