Colorimetric Determination of Propofol in Bulk form,Dosage Form and Biological Fluids

ABSTRACT

Propofol is coupled with 2, 6-dichloroquinone-4-chlorimide (DCQ) in a reaction buffered at pH 9.6 to give a colored product having an analytically useful maximum at 635 nm. The factors affecting the color generation were optimized and incorporated in the procedure. The reacted propofol has a molar absorptivity of 3.9 × 10^?4 L mol^?1 cm^?1, and Beer's law is obeyed for concentrations 1-5 μg ml^?1 with detection limit 0.25 μg ml^?1. The method was found applicable to biological fluids (plasma and urine) spiked with propofol at concentration levels 1-5 μg ml^?1 for plasma and 1-5 μg 0.5 ml^?1 urine (less sensitivity is obtained with urine volumes above 0.5 ml) with detection limits 0.28 μg ml^?1 for plasma and 0.4 μg 0.5 ml^?1 urine. The average recovery for the commercial preparation (1% w/v propofol emulsion intravenous injection for infusion) was 99.54% with an RSD of 1.05%. The method was validated by an adopted HPLC method. The results obtained by the HPLC method for the commercial preparation were statistically compared with the proposed method and evaluated at the 95% confidence limits.     

ICP-AES and Colorimetry as Analytical Tools for the Determination of Phosphorus Containing Compounds,Including Phosphine

Abstract

The direct quantitative determination of phosphine in gaseous mixtures or in air samples is associated with a number of difficulties. the paper describes an alternative technique based on the oxidation of phosphine to phosphate. Phosphate can be analysed either by inductively coupled plasma-atomic emission spectrometry (ICP-AES) or by a colometric method.

Because the problem of a proper (quantitative) sampling of phosphine in the air of working environments and/or in gaseous mixtures is still unsolved, standard solutions of KH₂PO₄ have been used as analytes (“artifical samples”) in the ICP-AES method.

The statistics concerning the sample variances, obtained from the 2 methods mentioned above, indicate no differences.     

Colorimetric and Bromometric Determination of Pirbuterol Hydrochloride

Abstract

Two proposed methods are reported for the quantitation of pirbuterol hydrochloride, namely, (i) colorimetric and (ii) titrimetric methods. The colorimetric method is based on coupling betweem diazotized sulphanilamide and pirbuterol hydrochloride. Under the optimum conditions studied, the coupling product exhibits a maximum at 440 nm. Linear relation between absorbance, A, and concentration of pirbuterol hydrochloride is in the range 5–40 μgml^?1. The mean percentage obtained for capsules (Exirel^R ?15 mg) was 100.8 ± 0.7 whereas mean percentage recovery obtained for the authentic drug was 100.5 ± 0.8.

The titrimetric procedure involves bromination of authentic pirbuterol in acid medium and residual titration of excess bromine. The stoichiometry of the reaction was investigated and infra-red analysis, of the bromoderivative was carried out. When applied to capsules the bromometric method gave mean percentage of 100.18 ± 2.25.     

Colorimetric and Polarographic Methods of Analysis for Prenalterol Hydrochloride

Abstract

Two proposed methods have been described for the determination of prenalterol hydrochloride in acetate buffer (pH=4.1) as authentic material and in tablets form using a (i) colorimetric method based on reduction of ferric iron by prenalterol hydrochloride and subsequent measurement at 511 nm of the red color obtained by the treatment of the resultant ferrous iron with 1, 10-orthophenanthroline, (ii) a differential pulse polarographic method based on nitrosation with 0.1 M NaNO₂/dil. HC1 and consequent recording of the differential pulse polarogram. The differential polarogram was obtained under constant amplitude pulses of 50 mV (DP 50) superimposed on a linearly increasing DC-voltage ramp. The peak height (h), of the polarogram was measured at the peak potential of -0.2V on the dropping mercury electrode (DME) versus Ag/AgCl reference electrode. The linearity ranges observed are 0.6μgfml to 6.0μg/ml and 2μg/ml to 12μg/ml, respectively. The mean percentage recoveries for an authentic sample are 99.5±1.4 and 100.5±0.7, respectively. When applied to tablets claimed to contain 10 mg each, the mean percentages obtained are 99.7±2.3 and 100.6 ±1.5 respectively.     

相位梯度条纹假彩色化的色度研究

用色散单棱镜和双棱镜,对谱衍射干涉和傅里叶滤波准光干涉的相位梯度条纹,进行周期性非对称和对称假彩色编码.本文用色度学方法统一计算和分析了编码色的色品,主波长,色度纯,光度和单色含量与相位梯度的关系.导出了各种系统获得最佳编码色的结构参数条件.同时还提出了双棱镜非重叠色散相补的对称彩色编码新方法.     

Investigation of the iodine–poly(vinylpyrrolidone) interaction employed in the determination of biocidal iodine by colorimetric solid-phase extraction

Colorimetric solid-phase extraction (C-SPE) has been previously explored as a means to monitor the iodine-based disinfectant used in the water systems on board the space shuttle. This same disinfectant is baselined for eventual deployment in the US water recovery system planned for node 3 of the International Space Station (ISS). With C-SPE, the I₂ concentration is determined from the diffuse reflectance spectrum (DRS) of the yellow iodine–poly(vinylpyrrolidone) (PVP) complex using the Kubelka–Munk function. However, the solution chemistry of iodine is very complex and results in a variety of inorganic species (e.g., I⁻, I₂, I₃⁻, HOI) that have very different biocidal capabilities. Thus, the nature of the interaction of iodine with PVP, and more specifically, the identity of the iodine species involved in the interaction, requires more elucidation. This paper reports the findings from a series of detailed experiments conducted to elicit a more complete understanding of the iodine–PVP system employed in C-SPE. The results indicate that I₂, one of the two dominant biocidal forms of iodine, is the species responsible for the analytical signal in our C-SPE platform. These findings lay the ground work for the planned development of a multiplexed iodine determination and speciation platform for in-flight analysis of spacecraft water samples.     

Direct colorimetric detection of copper(II) ions in sampling using diffusive gradients in thin-films

A novel binding phase was developed for use in diffusive gradients in thin-film (DGT) sampling for Cu(II) by employing methylthymol blue as a chelating and chromogenic agent. Methylthymol blue was adsorbed onto beads of Dowex 1 × 8 resin (200-400 mesh) and the resin beads were then immobilised onto an adhesive disc. Analysis of exposed binding discs by either UV-vis spectrophotometry or computer imaging densitometry provided robust quantification of adsorbed Cu(II) in the 0.2-1 μg cm⁻² range, allowing detection at μg L⁻¹ concentrations in the test solution (ca. 17 μg L⁻¹ for a 24 h deployment), and in good agreement with established DGT theory. The method was shown to be a potential replacement for binding phases based on Chelex 100 where a colorimetric response to a specific metal is desired.     

Improved model for improving the inter-instrument agreement of spectrocolorimeters

A proposal by Robertson slightly modified by Berns and Petersen, to use spectral differences to predict systematic errors in spectrophotometers has found limited success in practical application. Porter suggested a way to improve the level of agreement between standardizing laboratories based on the Berns and Petersen method but suggested using derivatives calculated from piecewise polynomial splines. He did not know it at the time, but such a model was already in use. That model now has over five years of successful field testing and this paper discloses how the model was developed, the efficiency with which it can reduce systematic errors and the kinds of errors that cannot presently be corrected by computational comparison of reflectance or transmittance factor readings. For instruments of the same basic design, this model will produce a reduction of the systematic errors in colorimetric coordinates on the order of factors of 2–3. The magnitude of the initial color differences appears to be irrelevant. The corrective power of the model is limited by the numerical noise generated by the process of simulating analytical derivatives. We show that instruments with average color differences of 1.0 CIELAB unit can be reduced to a level of 0.5–0.3 units. Our testing has included a large variety of material samples including textiles, plastics, inks, paints and ceramics. Over 400 samples have been measured in proving this method. In addition, the model has been in place in industrial environments where multiple instruments of different manufacturer have been made to operate successfully from the same set of laboratory standards at reproducibility levels that rival those of national standards laboratories.     

应用吸光光度法测定液本有机产品的色度

根据色度学原理应用吸光光度法测定了工业乙酸酐及冰乙酸产品的色度。应用分光光度计,建立标准曲线,通过测定样品在380-780nm处的透光度,计算黄变度,查得其相应铂-钴色度号。此方法能准确地反映了样品的真实颜色,消除了人为误差,提高了分析方法的准确度。适用于日常工业分析、科学研究及仲裁,对于目视比色时存在色调干扰的样品测定尤为重要。     

Colorimetric Estimation of Melatonin in Pharmaceutical Formulations

 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, λ_max 397 nm) by oxidation of the indol moiety in melatonin with potassium persulphate (method B, λ_max 450 nm) or by reduction of osmium (VIII) (method C, λ_max 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.