A reversed-phase HPLC method with fluorescence detection for the determination of the aflatoxins B1, B2, G1 and G2 in 42 animal feeds, comprising corn (16), soya bean meal (8), mixed meal (13), sunflower, wheat, canola, palm kernel, copra meals (1 each) was carried out. The samples were first extracted using acetonitrile:water (9:1), and was further cleaned-up using a multifunctional column. Optimum conditions for the extraction and chromatographic separation were investigated. By adopting an isocratic chromatographic system using a mobile phase comprising acetonitrile:methanol:water (8:27:65, v/v/v), the separation of the four aflatoxins was possible within 30 min. Recoveries for aflatoxins B1, B2, G1 and G2 were 98 ± 0.7%, 95 ± 1.0%, 94 ± 3.6% and 97 ± 4.3%, respectively. The results show that eight samples (19%) were contaminated with aflatoxins, ranging from 6.5 to 101.9 ng g−1. Total aflatoxin levels in three samples exceed the legal limits of many countries of 20 ng g−1.
A simple analytical method was used in the present work for the simultaneous quantification of Ciprofloxacin and Isoniazid in pharmaceutical preparations. UV-Visible spectrophotometry has been applied to quantify these compounds in pure and mixture solutions using the first-order derivative method. The method depends on the first derivative spectrophotometry using zero-cross, peak to baseline, peak to peak and peak area measurements. Good linearity was shown in the concentration range of 2 to 24 µg∙mL-1 for Ciprofloxacin and 2 to 22 µg∙mL-1 for Isoniazid in the mixture, and the correlation coefficients were 0.9990 and 0.9989 respectively using peak area mode. The limits of detection (LOD) and limits of quantification (LOQ) were
... Show MoreA spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and l
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected opti
... Show MoreSimple, precise and economic batch and flow injection analysis (FIA)-spectrophotometric methods have been established for simultaneous determination of salbutamol sulfate (SLB) in bulk powder and pharmaceutical forms. Both methods based on diazotization coupling reaction of SLB with another drug compound (sulfadimidine) as a safe and green diazotization agent in alkaline medium. At 444 nm, the maximum absorption of the orange azo-dye product was observed. A thorough investigation of all chemical and physical factors was conducted for batch and FIA procedures to achieve high sensitivity. Under the optimized experimental variables, SLB obeys Beer’s law in the concentration range of 0.25-4 and 10-100 μg/mL with limits of detection of 0.0
... Show MoreSimple, precise and economic batch and flow injection analysis (FIA)-spectrophotometric methods have been established for simultaneous determination of salbutamol sulfate (SLB) in bulk powder and pharmaceutical forms. Both methods based on diazotization coupling reaction of SLB with another drug compound (sulfadimidine) as a safe and green diazotization agent in alkaline medium. At 444 nm, the maximum absorption of the orange azo-dye product was observed. A thorough investigation of all chemical and physical factors was conducted for batch and FIA procedures to achieve high sensitivity. Under the optimized experimental variables, SLB obeys Beer’s law in the concentration range of 0.25-4 and 10-100 μg/mL with limits of detection o
... Show MoreThis article aims to determine the time-dependent heat coefficient together with the temperature solution for a type of semi-linear time-fractional inverse source problem by applying a method based on the finite difference scheme and Tikhonov regularization. An unconditionally stable implicit finite difference scheme is used as a direct (forward) solver. While by the MATLAB routine lsqnonlin from the optimization toolbox, the inverse problem is reformulated as nonlinear least square minimization and solved efficiently. Since the problem is generally incorrect or ill-posed that means any error inclusion in the input data will produce a large error in the output data. Therefore, the Tikhonov regularization technique is applie
... Show MoreTwo simple, rapid, and useful spectrophotometric methods were suggest or the determination of sulphadimidine sodium (SDMS) with and without using cloud point extraction technique in pure form and pharmaceutical preparation. The first method was based on diazotization of the Sulphdimidine Sodium drug by sodium nitrite at 5 ºC, followed by coupling with α –Naphthol in basic medium to form an orange colored product . The product was stabilized and its absorption was measured at 473 nm. Beer’s law was obeyed in the concentration range of (1-12) μg∙ml-1. Sandell’s sensitivity was 0.03012 μg∙cm-1, the detection limit was 0.0277 μg∙ml-1, and the limit of Quantitation was 0.03605μg
... Show MoreBeta-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 chr
... Show MoreThis study was undertaken to introduce a fast, accurate, selective, simple and environment-friendly colorimetric method to determine iron (II) concentration in different lipstick brands imported or manufactured locally in Baghdad, Iraq. The samples were collected from 500-Iraqi dinars stores to establish routine tests using the spectrophotometric method and compared with a new microfluidic paper-based analytical device (µPAD) platform as an alternative to cost-effective conventional instrumentation such as Atomic Absorption Spectroscopy (AAS). This method depends on the reaction between iron (II) with iron(II) selective chelator 1, 10-phenanthroline(phen) in the presence of reducing agent hydroxylamine (HOA) and sodium acetate (NaOAc) b
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