A simple, sensitive and accurate method has been developed for spectrofluorimetric determination of cefixime in pure form and pharmaceutical preparations. The method is based on the reaction of cefixime with 2-cyanoacetamide in the presence of 21% ammonia at 100 °C. The fluorescent reaction product showed maximum fluorescence intensity at λ 378 nm after excitation at λ 330 nm. The factors affecting the derivatization reaction were carefully studied and optimized. The fluorescence intensity versus concentration plot was rectilinear over the range of 0.02 to 4 μg mL(-1) with correlation coefficient of 0.99036. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 2.95 ng mL(-1) and 9.84 ng mL(-1), respectively. The proposed method was validated statistically and through recovery studies. The method was successfully applied for the determination of cefixime in pure and dosage form with percent recoveries from 98.117% to 100.38%. The results obtained from the proposed method have been compared with the official HPLC method and good agreement was found between them.
We describe the development and validation of a new, simple, sensitive and cost-effective method for the determination of ceftriaxone in commercial formulations and spiked human plasma. The method proposes the conversion of ceftriaxone into a fluorescent product by reacting with ortho-phthalaldehyde (OPA) in the presence of sulfite at room temperature. The reaction medium is buffered to pH 10 using borate buffer. The derivatized reaction product is highly fluorescent and exhibits maximum fluorescence intensity at λ(em) = 386 nm after excitation at λ(ex) = 324 nm. The experimental parameters affecting progress of the derivatization reaction were carefully studied and optimized. Under optimum experimental conditions, the method has an excellent correlation coefficient of 0.9984 with a broad linear range of 0.4-20 µg/mL. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 1.30 × 10(-3) and 3.90 × 10(-3) µg/mL, respectively. The interference effects of common excipients on the quantification of drug were investigated and no interference effect was observed. The proposed method has been successfully applied to the determination of ceftriaxone in pharmaceutical formulations and spiked human plasma samples. The method has been validated statistically through percent recovery studies using standard addition and by comparison with a reference HPLC method. The developed method exhibits excellent inter- and intraday precision.
A new spectrofluorimetric method has been developed and validated for the quantification of ceftriaxone in bulk powder, pharmaceutical formulations and spiked human plasma. The developed method is reproducible, accurate, sensitive and cost effective. In this method, ceftriaxone was converted into a fluorescent compound by reacting with 0.8 M ethyl acetoacetate and 25% formaldehyde in a buffered medium (pH = 4.2) at 90 °C. The excitation and emission wavelengths of the fluorescent reaction product are 316 nm and 388 nm respectively. Optimization of the experimental conditions affecting the condensation reaction were carefully carried out and the optimum experimental conditions were incorporated in the procedure. The developed method has a broad linear range (0.2-20 μg mL(-1)) with a correlation coefficient of 0.9992. The limit of detection (LOD) and limit of quantification (LOQ) was found to be 1.94 × 10(-2) μg mL(-1) and 6.47 × 10(-2) μg mL(-1) respectively. The common excipients and co-administered drugs were investigated for their interferences effect in the assay. The developed method was validated statistically through recovery studies and successfully applied to ceftriaxone determination in bulk powder, pharmaceutical formulations and spiked human plasma samples. The percent recoveries were found to be in the range of 99.04-100.26% for bulk powder, 98.88-99.92% for pharmaceutical formulations and 94.22-98.48% for spiked human plasma. The results were verified by comparing with reference literature HPLC method and were found in good agreement.
Two simple, sensitive and accurate spectrofluorimetric and spectrophotometric methods have been developed for the determination of sparfloxacin in bulk and pharmaceutical preparations. The proposed methods were based on oxidation of sparfloxacin with Ce (IV) in acidic medium. The spectrophotometric method involved the measurement of unconsumed Ce (IV) concentration at 315 nm. The spectrofluorimetric method based on the measurement of reduced fluorescent Ce (III) at 352 nm after excitation at 250 nm. Different variables affecting the reaction such as concentration and volume of cerium (IV), type and concentration of acidic medium, heating temperature and time were carefully studied and optimized. Under the optimum conditions, linear relationship in the range of 0.02-0.2 μg mL<sup>-1</sup> and 0.02-0.1 μg mL<sup>-1</sup> were obtained using spectrophotometric and spectrofluorimetric methods, respectively. No interferences were observed from the common formulations excipients present in the dosage form of the drug. The proposed methods were successfully applied to the analysis of the investigated drug in pure and pharmaceutical formulations with good accuracy and precision. The recovery percentage ranged from 93-102 ± 1.73-2.66%. The precision of the methods were good; RSD ≤ 2.55%.
A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of cefaclor and ceftriaxone cephalosporin antibiotic. The developed method has been validated and applied to mixtures of the commercial formulation and spiked human plasma. A mediterranea C<sub>18</sub> column (4.6 × 250 mm) was used with isocratic solvent delivery system and UV-visible detector. Different experimental parameters like solvent composition (acetonitrile: methanol: triethyl amine buffer 1:1:2 (v/v), flow rate of mobile phase (0.6 mLmin<sup>-1</sup>), pH of the buffer (7), and wavelength (260 nm) were optimized for effective separation and esolution of the analyte peaks. The separation was achieved in 6 min with retention times of 4.94 ± 0.056 min and 3.39 ± 0.022 min for cefaclor and ceftriaxone respectively. The linear range for both the studied drugs was found to be 0.5-250 μgmL<sup>-1</sup> with r<sup>2</sup> of 0.9987 (cefaclor) and 0.9997 (ceftriaxone). The limit of detection (3.3 σ/S) was found to be 2.34 × 10<sup>-2</sup> μgmL−1 and 1.70 × 10−2 μgmL<sup>-1</sup>, respectively, for cefaclor and ceftriaxone. Similarly limit of quantification (10σ/S) was 7.10 × 10−2 μgmL<sup>-1</sup> for cefaclor and 5.15 × 10−2 μgmL<sup>-1</sup> for ceftriaxone. The chromatographic procedure was applied to commercial formulations and spiked human plasma and the results were compared with literature HPLC method.
A sensitive spectrofluorimetric method was developed for determination of ciprofloxacin (CPFX), levofloxacin (LEV), gatifloxacin (GAT) and moxifloxacin (MOX) in pure, commercial formulations, human urine and plasma. The method is based on charge-transfer (CT) complex with chloranilic acid. Fluorescence intensity of the complexes was measured at emission wavelength ranging from 445 -492 nm with excitation wavelengths from 285 -330 nm. At optimum experimental conditions, a linear calibration plot was obtained in the concentration range of 20 -1000 ng·mL , 20 -800 ng·mL −1 and 20 -100 ng·mL −1 for CPFX, LEV, MOX and GAT, respectively with good correlation coefficient in the range of 0.9929 -1.0 in methanolic medium. The limit of detection and limit of quantification were found to be 5 ng·mL −1 and 18 ng·mL −1 for CPFX, 12 ng·mL −1 and 40 ng·mL −1 for LEV, 8 ng·mL −1 and 19 ng·mL −1 for MOX, 6 ng·mL −1 and 19 ng·mL −1 for GAT, respectively. The method was found free of interferences from excipients used as additive in pharmaceutical preparations, some common cations and compounds present in urine and plasma as well as co-administered analgesic, vitamins and other drugs. The method was successfully applied for quantification of selected fluoroquinolones in commercial formulations and also in spiked human urine and plasma samples with percent recoveries of 100.0 ± 1.56 and 100.2 ± 1.29 respectively.
Objective: The purpose of this study is to determine the functional and radiological outcomes of modified stoppa approach for fixation of acetabular fractures. Study Design: Descriptive Study Place and Duration: Study was conducted at Orthopaedic department of Ayub Teaching Hospital Abbottabad, Fauji Foundation Hospital, Rawalpindi and Islamabad International Hospital E-11/4, Islamabad for duration of two years form July 2019 to June 2021. Methods: There were thirty patients of both genders who had acetabular fractures were presented. Included patients were aged between 18-55 years. Patients' age, sex, body mass index and cause of fractures were recorded after taking informed written consent. Types of acetabular fractures were also recorded. Modified stoppa approach was used to operate acetabular fractures. Outcomes were operative time, radiological and functional outcomes were assessed in terms of excellent, good, fair and poor results. Post-operative complications and patients' satisfaction was also calculated. We used SPSS 24.0 version to analyze complete data. Results: Among 30 cases, majority of the patients 20 (66.67%) were males and 10 (33.33%) were females with mean age 29.4±10.37 years. Mean body mass index of the presented patients was 23.7±7.25 kg/m2. RTA was the most common cause found in 17 (56.67%), followed by fall from height in 8 (26.67%) and 5 (16.67%) fractures had other causes. Anterior wall fracture was the most common type found in 14 (46.67%) cases. Mean operative time was 3.87±13.18 hours. As per radiological outcomes, frequency of anatomical reduction found in 21 (73.3%) cases, not perfect found in 5 (16.67%) cases and poor results found in 4 (13.3%) patients. Majority of the cases 18 (60%) had good results in functional outcomes, excellent results in 7 (23.3%), fairs results in 3 (10%) cases and poor in 2 (6.67%) cases. Post-operative complications found in 2 (6.67%) cases. Satisfaction rate among patients was 86.67%. Conclusion: We found in this study that the use of stoppa approach for fixation of acetabular fractures was effective and safe method in terms of good radiological and functional outcomes. Except this less operative time and less number of complications were calculated with high number of customer’s satisfaction. Keywords: Acetabular Fractures, MSA, Complications, RTA
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