In this paper, turbidimetric and reversed-phase ultra-fast liquid chromatography (UFLC) methods were described for the quantitative determination of ephedrine hydrochloride in pharmaceutical injections form. The first method is based on measuring the turbidimetric values for the formed yellowish white precipitate in suspension status in order to determine the ephedrine hydrochloride concentration. The suspended substance is formed as a result of the reaction of ephedrine hydrochloride with phosphomolybdic acid which was used as a reagent. The physical and chemical characteristics of the complex were investigated. The calibration graphs of ephedrine were established by turbidity method. While the second method (UFLC) was conducted using the methanol-water (55+45, v/v) as the mobile phase with adjusted water pH 3.5. The ephedrine hydrochloride was detected and measured using UV detector at 260 nm. The linearity of ephedrine was obtained in the range of 0.09–0.39 mmol·l-1 . The detection limits (LOD) for the ephedrine hydrochloride were found to be 0.4 and 0.0044 mmol·l-1 by turbidity and UFLC, respectively. The developed methods were successfully applied for the quantitative determination of ephedrine hydrochloride in laboratory preparations (standard) and in commercial pharmaceutical injections. The two methods have given relative standard deviations (R.S.D.) in the range of 0.65–1.69 %, which indicates reasonable repeatability and high precision of both methods.
An easy, eclectic, precise high-Performance Liquid Chromatographic (HPLC) procedure was evolved and validated to estimate of Piroxicam and Codeine phosphate. Chromatographic demarcation was accomplished on a C18 column [Use BDS Hypersil C18, 5μ, 150 x 4.6 mm] using a mobile phase of methanol: phosphate buffer (60:40, v/v, pH=2.3), the flow rate was 1.1 mL/min, UV detection was at 214 nm. System Suitability tests (SSTs) are typically performed to assess the suitability and effectiveness of the entire chromatography system. The retention time for Piroxicam was found to be 3.95 minutes and 1.46 minutes for Codeine phosphate. The evolved method has been validated through precision, limit of quantitation, specificity,
... Show MorePesticides serve a crucial function in contemporary farming practices, safeguarding agricultural crops against pest infestations and boosting production outputs. However, indiscriminate use has caused environmental and human health damage. This study aimed to develop and validate a gas chromatography-flame ionization detection (GC-FID) methodology for the direct and routine analysis of spiromesifen residues in soil, leaves, and tomato fruits. The proposed method prioritizes simplicity by avoiding derivatization steps, offering advantages over existing approaches that utilize lengthy multi-step extraction or derivatization prior to GC analysis. A key novelty of this work is the development of a QuEChERS extraction coupled directly to GC-FID
... Show MoreAn Indirect simple sensitive and applicable spectrofluorometric method has been developed for the determination of Cefotaxime Sodium (CEF), ciprofloxacin Hydrochloride (CIP) and Famotidine (FAM) using reaction system bromate-bromide and acriflavine (AF) as fluorescent dye. The method is based on the oxidation of drugs with known excess bromate-bromide mixture in acidic medium and subsequent determination of unreacted oxidant by quenching fluorescence of AF. Fluorescence intensity of residual AF was measured at 528 nm after excitation at 402 nm. The fluorescence-concentration plots were rectilinear over the ranges 0.1-3.0, 0.05-2.6 and 0.1-3.8 µg ml-1 with lower detection limits of 0.013, 0.018 and 0.021 µg ml-1 an
... 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 MoreWe studied in this research how to find a method of estimating the quantity (Kinetically) of three kinds of Insecticide and their mixture, which are used in agriculture. The extracted insecticide from the polluted samples with these insect from air, soil, and the leaves of trees, have be used into the reaction with H2O2 and benzedine. The kinetic study of this reaction was formed in basic medium,( pH= 8.6), using UV. Spectra at (?= 420nm). The study showed that the reaction is the first order, and the speed of the reaction was used to estimate the concentration of insecticide in solution and mixture. The experiments of this study indicated that this method has the speed and efficiency for quantitatively estimating these
... Show MoreThe first flow injection spectrophotometric method is characterized by its speed and sensitivity which have been developed for the determination of promethazine-HCl in pure and pharmaceutical preparation. It is based on the in situ detection of colored cationic radicals formed via oxidation of the drug with sodium persulphate to pinkish-red species and the same species was determined by using homemade Ayah 3SX3-3D solar flow injection photometer. Optimum conditions were obtained by using the high intensive green light emitted diode as a source. Linear dynamic range for the absorbance versus promethazine-HCl concentration was 0-7 mmol.L-1, with the correlation coefficient (r) was 0.9904 while the percentage linearity (r2%) was 98.09%. the L.
... Show MoreA modern, rapid RP-HPLC-UV method was developed and validated in compliance with FDA and EMA guidelines for simultaneous quantification of 15 βlactam antibiotics) Ampicillin, Amoxicillin, cephalexin, cefotaxime, cefoxitin, cefamandole, cephalothin, piperacillin, penicillin, oxacillin, cloxacillin, nafcillin Carbenicillin, Mezlocillin and Dicloxacillin) in pharmaceutical formulations and pure forms. The method employs Column NEUCLEODUR C-18 (4.0 mm x 100 mm, 5µm particle size), at a temperature of thirty degrees Celsius, and the mobile phase was acetonitrile and KH2PO4 using gradient elution with a total separation time of 13 minutes, a flow rate of 1.3 ml/min, at = pH 4.5 for the buffer solution and the λ max was 220 nm. The met
... Show MoreA direct, sensitive and efficient spectrophotometric method for the determination of nitrofurantoin
drug (NIT) in pure as well as in dosage form (capsules) was described. The suggested method was
based on reduction NIT drug using Zn/HCl and then coupling with 3-methyl-2-benzothiazolinone
hydrazone hydrochloride (MBTH) in the presence of ammonium ceric sulfate. Spectrophotometric
measurement was established by recording the absorbance of the green colored product at 610 nm.
Using the optimized reaction conditions, beer’s law was obeyed in the range of 0.5-30 μg/mL, with
good correlation coefficient of 0.9998 and limits of detection and quantitation of 0.163 and 0.544
μg/mL, respectively. The accuracy and