Optimization of high-performance liquid chromatographic parameters for the determination of capsaicinoid compounds using the simplex method.

A high-performance liquid chromatographic method was developed for the analysis of capsaicinoid compounds, the pungent principles of capsicum fruits. A sequential simplex method was applied to optimize the chromatographic response function used to assess the quality of separation by varying the chromatographic parameters. The separation was achieved in 11 min using a C-8 column of 15-cm length and 4.6 mm diameter using a UV detector. A flow rate of 1.15 ml min(-1) at a column temperature of 43.5 degrees C using 63.7% methanol in water gave the most efficient separation. The method was found to be suitable for the determination of the major capsaicinoid compounds in the capsicum samples.     

Metallosurfactants: interfaces and micelles

Incorporating a metal cation as an integral component of the headgroup of a surfactant--a metallosurfactant--offers a route to concentrate these ions and their associated functionality at interfaces. To reduce the lability of the metal, various chelating or macrocyclic ligands may be employed leading to a family of homologous series of related metallosurfactants with a structural diversity that is arguably broader than is inherently possible with conventional surfactants. This review discusses the small number of key papers that are quantifying the physico-chemical properties of metallosurfactants and highlights their "classical" as well as "non-classical" surfactant behaviour, providing an insight into the structure of micelles and films formed from these novel materials.     

Separation of some transition-metal ions on silica-immobilized 2-pyridinecarboxaldehyde phenylhydrazone

A metal-ion extractant, prepared by chemical binding of 2-pyridinecarboxaldehyde phenylhydrazone on a silica support, is described and shown to be effective for use in separation and determination of trace amounts of iron, cobalt, nickel, and copper. Metal-ion sorption conforms to the Langmuir isotherm. The relative orders of the Langmuir constants K and the column retention-capacity factors k' for the four transition-metal ions are the same as the natural order of the stabilities predicted for their metal chelates: Fe(II) < Co(II) < Ni(II) < Cu(II).     

Reverse flow injection spectrophotometric determination of iron(III) using norfloxacin

A reversed flow injection colorimetric procedure for determining iron(III) at the μg level was proposed. It is based on the reaction between iron(III) with norfloxacin (NRF) in 0.07 mol l⁻¹ ammonium sulfate solution, resulting in an intense yellow complex with a suitable absorption at 435 nm. Optimum conditions for determining iron(III) were investigated by univariate method. The method involved injection of a 150 μl of 0.04% w/v colorimetric reagent solution into a merged streams of sample and/or standard solution containing iron(III) and 0.07 mol l⁻¹ ammonium sulfate in sulfuric acid (pH 3.5) solution which was then passed through a single bead string reactor. Subsequently the absorbance as peak height was monitored at 435 nm. Beer's law obeyed over the range of 0.2–1.4 μg ml⁻¹ iron(III). The method has been applied to the determination of total iron in water samples digested with HNO₃–H₂O₂ (1:9 v/v). Detection limit (3σ) was 0.01 μg ml⁻¹ the sample through of 86 h⁻¹ and the coefficient of variation of 1.77% (n=12) for 1 μg ml⁻¹ Fe(III) were achieved with the recovery of the spiked Fe(III) of 92.6–99.8%.     

New approach to single-particle time-correlation function theory: Application to intramolecular dephasing in the condensed phase

A new approach to solve the linewidth expression of infrared line shape based on the Kim-Wilson single-particle time-correlation function theory is presented. A projection-operator technique coupled with an explicit series-expansion method is used to reduce the unusual operator exp[1(1 - P)Lt] in the damping function to the usual operator exp(i L⁰t). This approach is applied to a study of a temperature dependence of the width and shift of the infrared line shape for intramolecular dephasing of a polyatomic molecule in the condensed phase.     

Flow-injection spectrophotometric determination of calcium using murexide as a color agent

FI spectrophotometric determination of calcium using murexide has been developed. The problem of the color of the dye fading and/or its complex in an alkaline medium in the batch method can be overcome by taking advantage of FIA. A calcium solution is injected into an ethylenediamine–ethylenediamine hydrochloride buffer (1 M, pH 11) which also serves as a masking agent, and is then merged with the aqueous murexide (0.005%, w/v) and continuously monitored. Simple FIA manifolds, including an LED colorimeter detector hooked up to a PC-based data acquisition and evaluation system are described. Optimization of FIA systems has been made. The proposed procedures have been validated by using reference materials and comparing the results with the standard methods, and then applied to ores and drug samples.     

Flow injection spectrophotometric determination of tetracycline in a pharmaceutical preparation by complexation with aluminium(III).

A rapid flow injection (FI) spectrophotometric procedure for tetracycline determination is described. It is based on the injection of a 100 microl sample solution containing tetracycline into merged streams of aluminium(III) chloride (0.01 mol 1(-1)) and Tris-buffer in the presence of KCl (0.06 mol l(-1)), pH 7.0, with the same optimum flow rate of 3.2 ml min(-1). A yellow Al(III)-tetracycline complex was monitored at 376 nm. The flow injection system and the experimental conditions were optimized by means of the univariate method. The procedure was applied to the determination of tetracycline in pharmaceutical preparations with a high sampling rate of at least 165 h(-1). A high precision with a relative standard deviation was obtained less than 0.72 and 0.30% of 5.0 and 10 microg ml(-1) (n=11), respectively. The detection limit (3sigma) and the quantification limit (10sigma) were 0.07 and 0.72 mg l(-1), respectively. There were no interference effects from traditional excipients in the dosage forms when the method was applied to pharmaceutical preparations. The matrix effect could be reduced by the standard addition method.