Beta-lactam medications are among the commonly used antibiotics that share the presence of a beta-lactam ring in their chemical formation. A modern, rapid, highperformance liquid chromatography technique was advanced and validated according to FDA and EMA rules for the concurrent determination of medications in their pharmaceutical and pure forms This study deals with the determination of beta-lactam drugs )Amoxicillin, Ampicillin Cephalexin, Cefotaxime, Cefoxitin, Cefamandole, Cephalothin, Piperacillin, Penicillin, Oxacillin, Cloxacillin Nafcillin, Carbenicillin, Mezlocillin and Dicloxacillin) which is a RP-HPLC technique with an UV detector using a column NEUCLEODUR C-18 (4.0 mm × 100 mm, 5µm particle size), The heat of the chromatographic column was 30o C, and the mobile phase of acetonitrile and KH2 PO4 using a progression elution with a total separation time of 19.54 min, a flow rate of 1.3, and the wavelength was 220 nm. The concentration range was among (0.2–20 µg/ml) with coefficients of determination of 0.9994. Recoveries were 100.4 – 90.86%, the limit of detection (LOD) was 0.0069–0.0659 µg/ml and limit of quantitation (LOQ) was 0.0211–0.1997 µg/ml. The chromatography approach advanced in this study was applied to simultaneously identify drugs in medical dosage forms obtained from pharmacies.
Simple and sensitive kinetic methods are developed for the determination of Paracetamol in pure form and in pharmaceutical preparations. The methods are based on direct reaction (oxidative-coupling reaction) of Paracetamol with o-cresol in the presence of sodium periodate in alkaline medium, to form an intense blue-water-soluble dye that is stable at room temperature, and was followed spectrophotometriclly at λmax= 612 nm. The reaction was studied kinetically by Initial rate and fixed time (at 25 minutes) methods, and the optimization of conditions were fixed. The calibration graphs for drug determination were linear in the concentration ranges (1-7 μg.ml-1) for the initial rate and (1-10 μg.ml-1) for the fixed time methods at 25 min.
... Show MoreA rapid high performance liquid chromatography method for the determination of sphinganine (Sa) and sphingosine (So) in urine samples by employing a silica-based monolithic column is described. The samples were first extracted using ethyl acetate and derivatized using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol. C20 sphinganine was used as internal standard. Under the optimized conditions, separation was achieved using a mixture of methanol:water (93:7, v/v), column temperature at 30°C, flow rate of 1 mL min−1, and an injection volume of 10 μL. Good linearity was obtained for Sa and So over the concentration range 20–500 ng mL−1(correlation coefficients ≥0.9978). The detection limits were 0.45 ng mL−1 for Sa and
... Show MoreHigh-performance liquid chromatographic methods are used for the determination of water-soluble vitamins with UV-Vis. Detector. A reversed-phase high-performance liquid chromatographic has been developed for determination of water-soluble vitamins. Identification of compounds was achieved by comparing their retention times and UV spectra with those of standards solution. Separation was performed on a C18 column, using an isocratic 30% (v/v) acetonitril in dionozed water as mobile phase at pH 3.5 and flow rate 1.0m/min. The method provides low detection and quantification limits, good linearity in a large concentration interval and good precision. The detection limits ranged from 0.01 to 0.025µg/ml. The accuracy of the method was
... Show MoreAbstract :In this study, amygdaline in Iraqi plant seeds was extracted and isolated from their seeds matrix using reflux procedure and subsequently identified and determined by high performance liquid chromatography (HPLC) on reversed phase column of LC-18 (150mm x 4.6mm, 5?m )with actonitrile :water ( 50 : 50 ) as mobile phase at flow rate of ( 0.5 mL/min ) and detection at wavelength of 215 nm.The experimental results indicated that the linearity of calibration is in the range of 1.0-30.0 mg L-1amygdaline with the correlation coefficient of 0.9949. The limit of detection (LOD) and limit of quantitation (LOQ) for amygdaline were of 0.88 and 2.93 mg L-1 in standard pure sample. The mean recovery percent is 97.34±0.58 at 95% confidence inte
... Show MoreIn this study, simple, low cost, precise and speed spectrophotometric methods development for evaluation of sulfacetamide sodium are described. The primary approach contains conversion of sulfacetamide sodium to diazonium salt followed by a reaction with p-cresol as a reagent in the alkaline media. The colored product has an orange colour with absorbance at λmax 450 nm. At the concentration range of (5.0-100 µg.mL-1), the Beer̆ s Low is obeyed with correlation coefficient (R2= 0.9996), limit of detection as 0.2142 µg.mL-1, limit of quantification as 0.707 µg.mL-1 and molar absorptivity as 1488.249 L.mol-1.cm-1. The other approach, cloud point extraction w
... Show MoreThe most hazardous class of pharmaceuticals for soil and aquatic ecosystems are antibiotics, which include prescription medications and cancer treatments. Hospital effluents are usually produced by all parts of medical facilities, including hospitals. This study's specific goal was to provide a quick, affordable, and accurate analytical technique for determining the levels of amoxicillin, azithromycin, and penicillin in wastewater from Medical City, Al-Mahmudiya, and Al-Yarmouk hospitals (Iraq, Baghdad). An HPLC with a receptive ODS C18 column was used. It was equipped with UV and pulsed amperometric detectors with wavelengths of 230 nm and 210-240 nm, respectively. The correlation coefficients for each drug are greater than 0.9999,
... Show MoreThe current study performed in order to detect and quantify epicatechin in two tea samples of Camellia sinensis (black and green tea) by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). Extraction of epicatechin from black and green tea was done by using two different methods: maceration (cold extraction method) and decoction (hot extraction method). Qualitative and quantitative determinations of epicatechin in two tea samples were investigated. Epicatechin identification was made by utilizing preliminary chemical tests and TLC. This identification was also boosted by HPLC and then quantified epicatechin in all ethyl acetate fractions of two tea samples. This research revealed the existence of epica
... Show MoreThe current study performed in order to detect and quantify epicatechin in two tea samples of Camellia sinensis (black and green tea) by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). Extraction of epicatechin from black and green tea was done by using two different methods: maceration (cold extraction method) and decoction (hot extraction method) involved using three different solvents which are absolute ethanol, 50% aqueous ethanol and water for both extraction methods using room temperature and direct heat respectively. Crude extracts of two tea samples that obtained from two methods were fractionated by using two solvents with different polarity (chloroform and
... Show MoreA new, Simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sulfamethoxazole (SMZ) drug in pure and dosage forms. This method based on the reaction of sulfamethoxazole (SMZ) with 1,2-napthoquinone-4-sulphonic acid (NQS) to form Nalkylamono naphthoquinone by replacement of the sulphonate group of the naphthoquinone sulphonic acid by an amino group. The colored chromogen shows absorption maximum at 460 nm. The optimum conditions of condensation reaction forms were investigated by (1) univariable method, by optimizing the effect of experimental variables (different bases, reagent concentration, borax concentration and reaction time), (2) central composite design (CCD) including the effect of
... Show MoreIn this work, a simple and very sensitive cloud point extraction (CPE) process was developed for the determination of trace amount of metoclopramide hydrochloride (MTH) in pharmaceutical dosage forms. The method is based on the extraction of the azo-dye results from the coupling reaction of diazotized MTH with p-coumaric acid (p-CA) using nonionic surfactant (Triton X114). The extracted azo-dye in the surfactant rich phase was dissolved in ethanol and detected spectrophotometrically at λmax 480 nm. The reaction was studied using both batch and CPE methods (with and without extraction) and a simple comparison between the two methods was performed. The conditions that may be affected by the extraction process and the sensitivity of m
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