Rapid high-performance liquid chromatographic determination with fluorescence detection of furosemide in human body fluids and its confirmation by gas chromatography—mass spectrometry (original) (raw)
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Journal of Chromatography B, 2002
Furosemide, a drug that promotes urine excretion, is used in the pharmacotherapy of various diseases and is considered as a doping agent in sports. Using alkaline electrolytes, analysis of furosemide by dodecyl sulfate based micellar electrokinetic capillary chromatography (MECC) and capillary zone electrophoresis (CZE) with laser-induced fluorescence detection (LIF, analyte excitation with the 325 nm line of a HeCd laser) is described. Data produced by injection of plain or diluted patient urines are confirmed with those obtained via analysis of urinary solid-phase extracts. CZE-LIF and MECC-LIF are thereby shown to permit unambiguous recognition of furosemide in urines collected after ingestion of therapeutic doses of this drug. This is in contrast to solute detection via UV absorbance for which the extraction of furosemide is required. MECC based electropherograms are somewhat more complex compared to those obtained by CZE-LIF, this suggesting that the latter approach is more suitable for rapid screening of urines with direct sample injection and LIF detection. Alternatively, 2 capillary electrophoresis with negative electrospray ionization-ion-trap tandem mass spectrometry (CE-MS ) is shown to permit the direct confirmation of furosemide in human urine. This approach is based upon the monitoring of the m /z 2 329.3→m /z 285.2 precursor-product ion transition. CZE-LIF and CE-MS with injection of plain or diluted urine represent simple, rapid and attractive urinary screening and confirmation assays for furosemide in patient urines.
ANALYTICAL DETERMINATION OF FUROSEMIDE: THE LAST RESEARCHES
Furosemide (FUR) is an anthranilic acid derivative which is a potent diuretic widely used in the treatment of congestive heart failure and edema. FUR works by blocking the absorption of salt and fluid in the kidney tubules, causing a profound increase in urine output (diuresis). Due to the considerable use of FUR, analytical determination is frequent. In this manuscript, a review of the methods developed for determination of FUR from the year 2008 is presented.
Determination of Furosemide in Whole Blood using SPE and GC-EI-MS
Journal of Analytical Toxicology, 2005
A simple and rapid method was validated to determine furosemide in whole blood. The experimental work was performed so that all validation parameters are considered simultaneously in a one-day assay protocol. A solid-phase extraction procedure using BondElut| Certify columns was used to extract this compound from blood samples, while ketoprofen was used as an internal standard. The extracts were analyzed by gas chromatography-electron ionization-mass spectrometry after on-column derivatization with trimethylanilinium hydroxide (0.2M in methanol). Calibration curves were prepared daily, between 0.10 and 5.00 pg/mL, and the correlation coefficients were above 0.9910. The calculated limits of detection and quantitation were 0.010 and 0.045 pg/mL, respectively. Control samples at low, medium, and high concentrations (0.30, 0.75, and 3.00 pg/mL) of furosemide of an independent source were measured in the same day. Precision and trueness, calculated in terms of relative standard deviation (%), were less than 15% for all concentration levels. The relative recoveries calculated for the three levels of the control samples were 104%, 89%, and 91%, respectively. In general, a sensitive, specific, and reliable procedure has been developed for the determination of furosemide in whole blood samples and was found suitable for the application in postmortem forensic toxicology routine analysis.
Ibn AL- Haitham Journal For Pure and Applied Science, 2018
Simple and rapid spectrophotometric determination of furosemide (FUR) has been investigated .The method is based on acid hydrolysis of FUR to free primary aromatic amine and diazotization followed by coupling with 3, 5 di methyl phenol (3, 5-DMPH) at basic medium. The absorbance was measured at 434 nm, the method was optimized for best condition, and beers' law is obeyed over the range of 0.4-50 µg.mL-1 with molar absorptivity and sandal's sensitivity 1.3899 x10 4 L moL-1 .cm-1 and 0.0238x10 4 µg.cm-2 respectively. Analysis of solution containing nineteen different concentrations of FUR gave a correlation coefficient of (0.9999) and limit of detection, limit of quantitation were 0.127, 0.464µg.mL-1 respectively. The reaction stoichiometry was evaluated by Job's and mole ratio method was found to be 1:1(diazotized FUR: 3, 5-DMPH) .The method was applied in synthetic urine and pharmaceutical formulation. The recovery of FUR in spiked urine was satisfactory resulting in the values of (99±3.32) %, the results of the suggested method was compared with available official literature method.
Journal of Natural Remedies
The low cost added to easy access and expectation of low or no side effects make these products increasingly attractive. When a product of natural origin contains synthetic substances that are not declared in its formulation, the synthetic substance is characterized as adulteration. In order to identify and quantify adulterants in natural products, analytical methods have been developed and used as fundamental tools in the control of these products. Thus, two products of natural origin indicated for treatment of rheumatic and inflammatory diseases were analyzed to verify the presence of the co-adulterant furosemide. Co-adulterant presence in the products was tested using an Agilent® brand 1100 HPLC system with a quaternary pump, an automatic injector and a DAD detector, with a mobile phase composed of methanol/formic acid 0.2% 60/40 (v/v). HPLC-DAD indicates the presence of the undeclared furosemide compound in the original formulation of both analyzed samples. In sample A, 24 mg of furosemide per gram was found, while in sample B, 47mg per gram of product was obtained. The consumption of adulterated products may lead to risks such as drug interaction and intoxication, since active ingredients of synthetic origin are added without taking in consideration adjustments and quality of the raw material.
An accurate, simple, fast and cheap spectrophotometric method has been developed for the determination of Furosemide (FUR) in pharmaceutical pure and dosage forms. The method is based on the reaction of 2,4- Di hydroxyl Benz aldehyde (DHBA) with Furosemide in the presence of Ethyl alcohol. This reaction produces a complex yellow colored product which absorbs maximally at 430 nm. Beer’s law was obeyed in the range of 3.3 – 82.69 μg/mL with molar absorptivity of 1.749×103 L mole-1 cm-1 Sandell’s sensitivity 0.11 μg.cm-2. The effects of variables such as temperature, concentration of color producing reagent, and stability of color were investigated to optimize the procedure. The results are validated statistically. The proposed method was applied to commercially available tablets, and the results were Pharmaceutical formulations.
Journal of Pharmaceutical Research International
Aims: Design of technical methods for the determination of Furosemide in its pure and pharmaceutical dosage form using spectral methods. Study Design: planned and executed to estimate Furosemide by using Visible spectrophotometric in pure and pharmaceutical dosage form. Place and Duration of Study: Laboratory of Analytical Research, chemistry department, college of Science, University of Mosul ,Mosul-Iraq, during the period of April 2021 to August 2021. Methodology: Furosemide, the commercially known drug Lazix, which is important in the treatment of heart diseases and high blood pressure. This study was carried out using JASCO V – 630, double-beam computerized UV-Visible spectrophotometer, with 1 cm matched cell, and HANA pH meter was used for reported pH readings. Results: The reaction between Furosemide and bromo-phenol blue, xylenol orange, and chromazorol S. The decreasing in the intensity of the resulted colored complex was measured using bromo-phenol blue, xylenol orange, Whi...
Pharmaceutical methods, 2012
Three simple, accurate and sensitive spectrophotometric methods for the determination of finasteride in pure, dosage and biological forms, and in the presence of its oxidative degradates were developed. These methods are indirect, involve the addition of excess oxidant potassium permanganate for method A; cerric sulfate [Ce(SO4)2] for methods B; and N-bromosuccinimide (NBS) for method C of known concentration in acid medium to finasteride, and the determination of the unreacted oxidant by measurement of the decrease in absorbance of methylene blue for method A, chromotrope 2R for method B, and amaranth for method C at a suitable maximum wavelength, λmax: 663, 528, and 520 nm, for the three methods, respectively. The reaction conditions for each method were optimized. Regression analysis of the Beer plots showed good correlation in the concentration ranges of 0.12-3.84 μg mL-1 for method A, and 0.12-3.28 μg mL-1 for method B and 0.14 - 3.56 μg mL-1 for method C. The apparent molar ab...
Журнал аналитической химии, 2014
Sequential injection chromatography (SIC) is based on a stopped flow approach utilizing micro scale low pressure pump and selection valves coupled with micro scale fiber optic spectrometric devices. In the current communication, a new method for the estimation of furosemide (FSD) and amiloride (AMD) in tablet formulation exploiting SIC is reported. The method was reverse phase liquid chromatographic based. The separation was carried out onto C18 monolithic column (4.6 × 50 mm) with a mobile phase composition of 25 mM phosphate buffer (pH 4.0)-acetonitrile (65 : 35, v/v). Other conditions were: sample volume 30 μL, flow rate 30 μL/s and UV detection at 283 nm. The SIC method is eco friendly and cost effective. The volume of consumed mobile phase was 3.25 mL. The sample frequency was 24 samples/h. The assay also exhibited linear dynamic ranges of 10-100 µg/mL for FSD and 5-80 µg/mL for AMD. Acceptable intra and inter day precision (the RSD values were less than 2.2%) as well as accuracy (the recovery range was 97.5-98.4%) were obtained for concentrations over the range of the standard curves. The procedure was established for the purpose of quality control at a pharmaceutical laboratory.