Green UPLC method for estimation of ciprofloxacin, diclofenac sodium, and ibuprofen with application to pharmacokinetic study of human samples.

Investigation of a unique and fast method for the determination and separation of a mixture of three drugs viz., ciprofloxacin (CIP), Ibuprofen (IBU), and diclofenac sodium (DIC) in actual samples of human plasma. Also, the technique was used to look at their pharmacokinetics study. Hydrocortisone was chosen as the internal standard (IS). The drugs were chromatographically separated using an Acquity ultra-performance liquid chromatography UPLC ® BEH C18 1.7 µm (2.1 × 150 mm) column with a mobile phase composed of acetonitrile: water (65:35, v/v) adjusted to pH 3 with diluted acetic acid. Plasma proteins were precipitated with acetonitrile. The separated drugs ranged from 0.3 to 10, 0.2-11, and 1-25 µg/mL for CIP, IBU, and DIC, respectively. Calibration curves were discovered to achieve linearity with acceptable correlation coefficients (0.99%). Examination of quality assurance samples showed exceptional precision and accuracy. Following the successful application of this improved technique to plasma samples, the pharmacokinetic characteristics of each selected drug were evaluated using (UPLC) with UV detection at 210 nm. Two green metrics were applied, the Analytical Eco-scale and the Analytical GREEnness Calculator (AGREE). Separation was achieved in only 4-min analysis time. The method's validation agreed with the requirements of the FDA, and the results were sufficient.

A novel gallium oxide nanoparticles-based sensor for the simultaneous electrochemical detection of Pb2+, Cd2+ and Hg2+ ions in real water samples.

Differential pulse voltammetry (DPV) using gallium oxide nanoparticles/carbon paste electrode (Ga2O3/CPE) was utilized for the simultaneous detection of Pb2+, Cd2+ and Hg2+ ions. Ga2O3NPs were chemically synthesized and fully characterized by Fourier-transform infrared (FTIR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Through the assay optimization, electrochemical screening of different nanomaterials was carried out using the cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) in order to determine the best electrode modifier that will be implemented for the present assay. Consequently, various parameters such as electrode matrix composition, electrolyte, deposition potential, and deposition time were optimized and discussed. Accordingly, the newly developed sensing platform showed a wide dynamic linear range of 0.3-80 µM with detection limits (LODs) of 84, 88 and 130 nM for Pb2+, Cd2+ and Hg2+ ions, respectively. While the corresponding limit of quantification (LOQ) values were 280, 320 and 450 nM. Sensors selectivity was investigated towards different non-targeting metal ions, whereas no obvious cross-reactivity was obtained. Eventually, applications on real samples were performed, while excellent recoveries for the multiple metal ions were successfully achieved.

Adsorption properties of kaolinite-based nanocomposites for Fe and Mn pollutants from aqueous solutions and raw ground water: kinetics and equilibrium studies.

Raw kaolinite was used in the synthesis of metakaolinite/carbon nanotubes (K/CNTs) and kaolinite/starch (K/starch) nanocomposites. Raw kaolinite and the synthetic composites were characterized using XRD, SEM, and TEM techniques. The synthetic composites were used as adsorbents for Fe and Mn ions from aqueous solutions and natural underground water. The adsorption by the both composites is highly pH dependent and achieves high efficiency within the neutral pH range. The experimental adsorption data for the uptake of Fe and Mn ions by K/CNTs were found to be well represented by the pseudo-second-order kinetic model rather than the intra-particle diffusion model or Elovich model. For the adsorption using K/starch, the uptake results of Fe ions was well fitted by the second-order model, whereas the uptake of Mn ions fitted well to the Elovich model rather than pseudo-second-order and intra-particle diffusion models The equilibrium studies revealed the excellent fitting of the removal of Fe and Mn ions by K/CNTs and Fe using K/starch with the Langmuir isotherm model rather than with Freundlich and Temkin models. But the adsorption of Mn ions by K/starch is well fitted with Freundlich rather than Temkin and Langmuir isotherm models. The thermodynamic studies reflected the endothermic nature and the exothermic nature for the adsorption by K/CNTs and K/starch nanocomposites, respectively. Natural ground water contaminated by 0.4 mg/L Fe and 0.5 mg/L Mn was treated at the optimum conditions of pH 6 and 120 min contact time. Under these conditions, 92.5 and 72.5% Fe removal efficiencies were achieved using 20 mg of K/CNTs and K/starch nanocomposites, respectively. Also, K/CNTs nanocomposite shows higher efficiency in the removal of Mn ions as compared to K/starch nanocomposite.

Determination of residues of acetaminophen, caffeine, and drotaverine hydrochloride on swabs collected from pharmaceutical manufacturing equipment using HPLC in support of cleaning validation.

An HPLC method was developed for the simultaneous determination of residues of acetaminophen (paracetamol, PA), caffeine (CA), and drotaverine HCl (DH) on swabs collected from pharmaceutical manufacturing equipment surfaces. The challenge in cleaning validation is to develop analytical methods that are sensitive enough to detect traces of the active compounds remaining on the surface of pharmaceutical manufacturing equipment after cleaning. Chromatography was performed in the isocratic mode on a Hypersil C18 BDS column using the mobile phase 0.02 M tetrabutylammonium bisulfate-methanol (100 + 45, v/v) at 50°C with UV detection at 210 nm. The method was tested for specificity, linearity, LOD, LOQ, accuracy, and precision for determination of traces of the above-mentioned drugs. The time required for a single analysis was 12 min. The response was linear in the ranges of 6.900-52.100, 1.040-7.800, and 0.694-5.210 µg/mL for PA, CA, and DH, respectively.

Clinical experience with shock-wave lithotripsy using the Siemens Modularis Vario lithotripter.

PURPOSE: To assess the effectiveness of a lithotripter (Modularis Vario; Siemens, AG Healthcare, Munich, Germany) in the management of renal and ureteric stones. PATIENTS AND METHODS: In all, 1146 adult patients with renal or ureteric stones were treated at one urological centre using the latest model of the Modularis Vario lithotripter. The effectiveness of lithotripsy and re-treatment rate were assessed. Data were obtained on stone location, stone size, shock wave usage, success rate, and complications. RESULTS: Between May 2007 and November 2009, 698 patients with renal stones and 448 with ureteric stones underwent extracorporeal shock-wave lithotripsy (ESWL). The mean (SD) renal stone size was 12.8 (3.8) mm; a mean of 1.36 sessions was required, with a mean (SD) number of 3744 (1961) shocks delivered per renal stone. After 3 months, the success rate defined as the patient being stone-free or with residual fragments of <4 mm; for renal stones the rate was 91.1%, with a 6.9% complication rate in the form of steinstrasse and severe renal colic. The mean (SD) ureteric stone size was 10.4 (2.7) mm. A mean of 1.37 sessions was required, with a mean (SD) of 4551 (2467) shocks delivered for each ureteric stone. The success rate for ureteric stones was 89.5%, with a 5.6% complication rate. The overall efficiency quotient was 0.66. CONCLUSION: The Siemens Modularis Vario lithotripter is a safe and effective machine for treating renal and ureteric stones.

Vaginal flap re-enforcement of vesico-vaginal fistula repair.

INTRODUCTION AND HYPOTHESIS: Vesicovaginal fistula (VVF) is a distressing urologic disorder. We describe a new technique that adds a third layer of closure during vaginal repair of VVF. METHODS: Twenty female patients with low VVF were included. A circumferential incision was made around the fistula that was completely excised. A rectangular vaginal flap was created just proximal to the site of the fistula. After closure of the urinary bladder, the distal edges of the vaginal flap were dissected and it was mobilized and interposed between the bladder and the vagina. Then the vagina was closed. RESULTS: The mean follow-up was 16 +/- 9 months. All of the patients are dry. None of them had any added morbidity due to the procedure. There are no postoperative complications. CONCLUSIONS: Vaginal flap reinforcement during vaginal repair of VVF is a simple and effective technique with high success rate and no added complications.

Telomerase activity, cytokeratin 20 and cytokeratin 19 in urine cells of bladder cancer patients.

AIM OF THE STUDY: This work aims to search for markers suitable for the screening of bladder cancer, which should be specific, sensitive, reproducible, non-invasive and at acceptable cost. PATIENTS AND METHODS: The study included 50 patients diagnosed as bladder cancer (35 TCC, 15 SCC) of different stages and grades, 30 patients with various urothelial diseases, besides 20 apparently healthy subjects of matched age and sex to the malignant group. A random midstream urine sample was collected in a sterile container for the determination of telomerase by RT-PCR, keratin 19 by ELSA CYFRA 21-1 IRMA kit, keratin 20 by RT-PCR and immunohistochemical staining, and urine cytology. RESULTS: For all parameters (telomerase, K19, K20 and cytology) the malignant group was significantly different from both the benign and the control groups. None of the four studied parameters was correlated to the stage of the disease, and when it comes to grade, only K19 showed a significant positive correlation with grade both in TCC and SCC. When ROC curves for all parameters were compared, K19 had the largest area under the curve, and then comes K20. CONCLUSION: K 19 may be used as a biological marker for the diagnosis of bladder cancer. K19 could not be used for differential diagnosis of different types of bladder cancer, meanwhile it could be a marker for differentiation that decreases in less differentiated tumors. As a tumor marker, K20 reflects inability to differentiate tumor type or grade in TCC, while in SCC of the bladder it is correlated with the grade. As a method, RT-PCR is superior to immunostaining for the detection of bladder cancer, meanwhile K20 immunohistochemistry (IHC) results were much better than urine cytology as a bladder cancer screening test. Haematuria and inflammation reduced the specificity of telomerase assay, which reduced its validity as a tumor marker of bladder cancer. K19 and K20 are the best candidates as screening tests for the diagnosis of bladder cancer, representing the highest sensitivity and specificity, beside the radiological and histopathology. Meanwhile, telomerase, although it was a sensitive enough marker, it reflected a high false positive rate.