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DEVELOPMENT AND VALIDATION OF HIGHPERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE SIMULTANEOUS DETERMINATION OF ANTIBIOTICS IN THEIR PURE FORM AND PHARMACEUTICAL FORMS
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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.

Publication Date
Sun Dec 03 2017
Journal Name
Journal Of Babylon University
Spectrophotometric Determination of Sulfamethoxazole in Pure and Pharmaceutical Preparations Based on Condensation Reaction Method
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A 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

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Publication Date
Sun Jun 21 2020
Journal Name
Baghdad Science Journal
Spectrophotometer Determination of Cefixime in pure form and pharmaceutical preparation by Using Cloud point Extraction
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Two simple methods spectrophotometric were suggested for the determination of Cefixime (CFX) in pure form and pharmaceutical preparation. The first method is based without cloud point (CPE) on diazotization of the Cefixime drug by sodium nitrite at 5Cº followed by coupling with ortho nitro phenol in basic medium to form orange colour. The product was stabilized and measured 400 nm. Beer’s law was obeyed in the concentration range of (10-160) μg∙mL-1 Sandell’s sensitivity was 0.0888μg∙cm-1, the detection limit was 0.07896μg∙mL-1, and the limit of Quantitation was 0.085389μg∙mL-1.The second method was cloud point extraction (CPE) with using  Trtion X-114 as surfactant. Beer

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Publication Date
Sun Jun 02 2019
Journal Name
Baghdad Science Journal
Micro Spectrophotometric Determination and Cloud Point Extraction of Sulphadimidine Sodium in Pure form and Pharmaceutical Drug
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Two 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

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Publication Date
Sun Dec 03 2017
Journal Name
Baghdad Science Journal
Synthesis New Liquid Selective Electrodes of Ciprofloxacin Hydrochloride for Determination Ciprofloxacin in Pure form and Pharmaceuticals Preparation.
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New membrane electrodes for determination of ciprofloxacin hydrochloride were prepared depending on ciprofloxacin hydrochloride - phosphotungstic acid (CFH-PT) as an active material and these electrodes were made with three plasticizers: Di-octylphenylphosphonate(DOPH), Di-butyl phosphate (DBP)Tri-n-butyl phosphate(TBP), in PVC matrix. One of the ciprofloxacin electrodes was gave Nernstian slope equal to 57.21 mV/ decade for DOPH membrane with concentration range from 1.5×10-5 to1.0×10-1 M, and detection limit equal to 1.5×10-6 M .Lifetime was 93 days. Non- Nernstian responses equal to 39.40 and 30.70 mV/ decade for membranes DBP, TBP, respectively. These electrodes were gave concentration range from 1.0× 10-5 to 1.0×10-2 and from 4.0

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Publication Date
Fri Dec 23 2022
Journal Name
Iraqi Journal Of Pharmaceutical Sciences ( P-issn 1683 - 3597 E-issn 2521 - 3512)
Sensitive Cloud Point Extraction Method for the Determination of Isoxsuprine Hydrochloride in Pharmaceutical forms using Spectrophotometry
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      A 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

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Publication Date
Fri Dec 23 2022
Journal Name
Iraqi Journal Of Pharmaceutical Sciences ( P-issn 1683 - 3597 E-issn 2521 - 3512)
Sensitive Cloud Point Extraction Method for the Determination of Isoxsuprine Hydrochloride in Pharmaceutical forms using Spectrophotometry
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      A 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 optimum conditions,

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Publication Date
Thu Dec 01 2022
Journal Name
Baghdad Science Journal
Simultaneous Ratio Derivative Spectrophotometric Determination of Paracetamol, Caffeine and Ibuprofen in Their Ternary Form
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A new, accurate, precise and economic two spectrophotometric methods for determination of Paracetamol (Par), Ibuprofen (Ibu), and Caffeine (Caf) were suggested. Those methods were the first and second ratio derivative spectrum using a double devisor. Par, Ibu, and Caf showed many useful peaks for their quantified determination. The validity of all analysis modes for determination of the three compounds, peak to baseline, peak area and peak to peak were according to ICH. The linearity of two methods was between 5 µg/ml as a lower concentration and 50 µg/ml as the highest concentration for three compounds. Recovery percentage was around 100% and relative standard deviation was less than 2.6%. The methods were applied successfully in the

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Publication Date
Thu Jan 06 2022
Journal Name
Chemical Papers
A solvent collection technique using dispersive liquid–liquid microextraction coupled with spectrophotometry for the trace determination of folic acid in pure, dosage forms and flaxseed
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A simple, rapid and environmentally friendly dispersive liquid–liquid microextraction method-based spectrophotometric method for the trace determination of folic acid has been developed. The proposed method is based on the formation of a deep yellow product via reaction of folic acid and 1,2-naphthoquine-4-sulfonate at pH = 9. The formed complex was extracted using a mixture of chloroform and ethanol. Then, the tiny organic droplets were measured at λ = 520 nm. At the optimum conditions, linearity was ranged from 0.05 to 1.5 μg/mL for the standard and samples, with a linear correlation coefficient of 0.9996. The detection limits were 0.02, 0.027, 0.03, 0.02 and 0.04 μg/mL for standard, tablet (5 mg), tablet (1 mg), syrup and fl

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Publication Date
Fri Nov 11 2022
Journal Name
Al-nisour Journal For Medical Sciences
Spectrophotometric determination of sulfamethoxazole in pure and pharmaceutical formulations
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New, easy, simple, and fast spectral method for estimation of sulfamethoxazole (SMZ) in pure and pharmaceutical forms. The proposed method is based on the azotization of the drug compound by sodium nitrite in an acidic medium and then coupling with 2,3dimethyl phenol reagent (DMP) in a basic medium to yield an orange-coloured dye which shows λmax at 402 nm. Different affection of the optimization reaction has been completed, following the classical univariate sequence. The concentration of sulfamethoxazole about (1-15) μg. mL-1 with molar absorptivity of (14943.461) L.mol1 .cm-1 that obeyed Beer’s law. The detection and quantification limits were (0.852, 2.583) μg. mL-1 respectively, while the value of Sandell’s sensitivity (

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Publication Date
Mon Dec 15 2025
Journal Name
Amecj
Rapid analysis and separation of fifteen beta-lactam drugs using reversed-phase high-performance liquid chromatography
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Beta-lactam medications are among the commonly used antibiotics. These drugs kill germs by disrupting cell wall formation. This drug treats bacterial infections in numerous body sections. A new, quick, high-performance liquid chromatography approach has been developed and verified by the FDA and EMA for the simultaneous estimation of drugs in their medicinal 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, Dicloxacillin) by a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) technique based on an UV detector using a

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