scholarly journals Development of the UV Spectrophotometric Method of Azithromycin in API and Stress Degradation Studies

2016 ◽  
Vol 68 ◽  
pp. 48-53 ◽  
Author(s):  
Sandip Bhimani ◽  
Gaurav Sanghvi ◽  
Trupesh Pethani ◽  
Gaurav Dave ◽  
Vishal Airao ◽  
...  
Keyword(s):  
Linear Relationship ◽  
Spectrophotometric Method ◽  
Phosphate Buffer ◽  
Macrolide Antibiotic ◽  
Limit Of Detection ◽  
High Sensitivity ◽  
Limit Of Quantification ◽  
Absorbance Maximum ◽  
Antibiotic Drug ◽  
Stress Degradation

Azithromycin (AZI) is a semi-synthetic macrolide antibiotic drug, effective against a wide variety of bacteria. The present study describes a simple, accurate, reproducible and precise UV Spectrophotometric method for the estimation of AZI (pH 6.8 Phosphate buffer). The absorbance maximum (λmax) for AZI was found to be 208nm. The method reveals high sensitivity, with linearity in the 10 µg/ml to 50 µg/ml range. The lower limit of detection was found to be 1.6µg/ml and the limit of quantification was found to be 5µg/ml. All the calibration curves demonstrated a linear relationship between the absorbance and concentration, with the correlation coefficient higher than 0.99. The % recovery was found to be 99.72%. AZI was also subjected to stress degradation under different conditions recommended by the International Conference on Harmonization (ICH).

scholarly journals APPLICATION AND VALIDATION OF DERIVATIVE SPECTROPHOTOMETRIC FOR DETERMINATION LEVELS OF TERNARY MIXTURES OF PARACETAMOL, PROPYPHENAZONE, AND CAFFEINE IN TABLET DOSAGE FORM

2018 ◽  
Vol 11 (13) ◽  
pp. 8
Author(s):  
Artha Yuliana Sianipar ◽  
Muchlisyam Muchlisyam ◽  
Siti Morin Sinaga
Keyword(s):  
Spectrophotometric Method ◽  
Phosphate Buffer ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Ternary Mixtures ◽  
Limit Of Quantification ◽  
Zero Crossing ◽  
Validation Parameters ◽  
Tablet Dosage ◽  
Third Derivative

 Objective: This study was to develop a spectrophotometric method with derivative zero-crossing for determines the levels of paracetamol (PCT), propyphenazone (PRO), and caffeine (CAF) in tablet dosage form without prior separation.Method: The study begins with optimizing the type of solvent, phosphate buffer (pH 7.2) and a mixture of phosphate buffer (pH 7.2) with methanol at ratio 90:10; 70:30; 50:50; 30:70; and 10:90. Spectrophotometric method with zero-crossing, tested validity based on linearity, accuracy, precision, limit of detection, and limit of quantification. Then, the method applied to determine the levels of PCT, PRO, and CAF in tablet.Result: The mixture of phosphate buffer (pH 7.2) with methanol at ratio 70:30 can be used for analysis. Applications zero-crossing technique on assay of PCT and CAF performed on the first derivative and Δλ 2 with λ 239.4 nm for PCT and Δλ 8 with λ 245.6 nm for CAF while PRO in the third derivative and Δλ 8 with λ 249.6 nm, resulting 100.91%, 104.75%, and 103.33% for levels of PCT, PRO, and CAF, respectively.Conclusion: Spectrophotometric derivative method with zero-crossing qualified in validation parameters.

scholarly journals DEVELOPMENT AND VALIDATION OF UV-SPECTROPHOTOMETRIC METHOD FOR ESTIMATION OF HYDROQUINONE IN BULK, MARKETED CREAM AND PREAPARED NLC FORMULATION

2017 ◽  
Vol 9 (5) ◽  
pp. 102
Author(s):  
Sukhjinder Kaur ◽  
Taranjit Kaur ◽  
Gurdeep Kaur ◽  
Shivani Verma
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Pure Form ◽  
Nanostructured Lipid Carrier ◽  
Limit Of Quantification ◽  
Double Beam ◽  
Uv Visible ◽  
Development And Validation

Objective: The aim of the present work was to develop a simple, rapid, accurate and economical UV-visible spectrophotometric method for the determination of hydroquinone (HQ) in its pure form, marketed formulation as well as in the prepared nanostructured lipid carrier (NLC) systems and to validate the developed method.Methods: HQ was estimated at UV maxima of 289.6 nm in pH 5.5 phosphate buffer using UV-Visible double beam spectrophotometer. Following the guidelines of the International Conference on Harmonization (ICH), the method was validated for various analytical parameters like linearity, precision, and accuracy robustness, ruggedness, limit of detection, quantification limit, and formulation analysis.Results: The obtained results of the analysis were validated statistically. Recovery studies were performed to confirm the accuracy of the proposed method. In the developed method, linearity over the concentration range of 5-40 μg/ml of HQ was observed with the correlation coefficient of 0.998 and found in good agreement with Beer Lambert’s law. The precision (intra-day and inter-day) of the method was found within official RCD limits (RSD<2%).Conclusion: The sensitivity of the method was assessed by determining the limit of detection and limit of quantification. It could be concluded from the results obtained that the purposed method for estimation of HQ in pure form, in the marketed ointment and in the prepared NLC-formulation was simple, rapid, accurate, precise and economical. It can be used successfully in the quality control of pharmaceutical formulations and for the routine laboratory analysis.

scholarly journals Quantification of Fosfomycin in Combination with Nine Antibiotics in Human Plasma and Cation-Adjusted Mueller-Hinton II Broth via LCMS

Antibiotics ◽  
2022 ◽  
Vol 11 (1) ◽  
pp. 54
Author(s):  
Kelvin Kau-Kiat Goh ◽  
Wilson Ghim-Hon Toh ◽  
Daryl Kim-Hor Hee ◽  
Edwin Zhi-Wei Ting ◽  
Nathalie Grace Sy Chua ◽  
...  
Keyword(s):  
Combination Therapy ◽  
Human Plasma ◽  
Limit Of Detection ◽  
Synergistic Activity ◽  
Limit Of Quantification ◽  
Mueller Hinton ◽  
Antibiotic Drug ◽  
Dosing Regimens ◽  
Antibiotic Combination

Fosfomycin-based combination therapy has emerged as an attractive option in our armamentarium due to its synergistic activity against carbapenem-resistant Gram-negative bacteria (CRGNB). The ability to simultaneously measure fosfomycin and other antibiotic drug levels will support in vitro and clinical investigations to develop rational antibiotic combination dosing regimens against CRGNB infections. We developed an analytical assay to measure fosfomycin with nine important antibiotics in human plasma and cation-adjusted Mueller–Hinton II broth (CAMHB). We employed a liquid-chromatography tandem mass spectrometry method and validated the method based on accuracy, precision, matrix effect, limit-of-detection, limit-of-quantification, specificity, carryover, and short-term and long-term stability on U.S. Food & Drug Administration (FDA) guidelines. Assay feasibility was assessed in a pilot clinical study in four patients on antibiotic combination therapy. Simultaneous quantification of fosfomycin, levofloxacin, meropenem, doripenem, aztreonam, piperacillin/tazobactam, ceftolozane/tazobactam, ceftazidime/avibactam, cefepime, and tigecycline in plasma and CAMHB were achieved within 4.5 min. Precision, accuracy, specificity, and carryover were within FDA guidelines. Fosfomycin combined with any of the nine antibiotics were stable in plasma and CAMHB up to 4 weeks at −80 °C. The assay identified and quantified the respective antibiotics administered in the four subjects. Our assay can be a valuable tool for in vitro and clinical applications.

scholarly journals Greener Monolithic Solid Phase Extraction Biosorbent Based on Calcium Cross-Linked Starch Cryogel Composite Graphene Oxide Nanoparticles for Benzo(a)pyrene Analysis

Molecules ◽  
2021 ◽  
Vol 26 (20) ◽  
pp. 6163
Author(s):  
Aree Choodum ◽  
Nareumon Lamthornkit ◽  
Chanita Boonkanon ◽  
Tarawee Taweekarn ◽  
Kharittha Phatthanawiwat ◽  
...  
Keyword(s):  
Graphene Oxide ◽  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
High Sensitivity ◽  
Rice Flour ◽  
Oxide Nanoparticles ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Significant Difference

Benzo(a)pyrene (BaP) has been recognized as a marker for the detection of carcinogenic polycyclic aromatic hydrocarbons. In this work, a novel monolithic solid-phase extraction (SPE) sorbent based on graphene oxide nanoparticles (GO) in starch-based cryogel composite (GO-Cry) was successfully prepared for BaP analysis. Rice flour and tapioca starch (gel precursors) were gelatinized in limewater (cross-linker) under alkaline conditions before addition of GO (filler) that can increase the ability to extract BaP up to 2.6-fold. BaP analysis had a linear range of 10 to 1000 µgL−1 with good linearity (R2 = 0.9971) and high sensitivity (4.1 ± 0.1 a.u./(µgL−1)). The limit of detection and limit of quantification were 4.21 ± 0.06 and 14.04 ± 0.19 µgL−1, respectively, with excellent precision (0.17 to 2.45%RSD). The accuracy in terms of recovery from spiked samples was in the range of 84 to 110% with no significant difference to a C18 cartridge. GO-Cry can be reproducibly prepared with 2.8%RSD from 4 lots and can be reused at least 10 times, which not only helps reduce the analysis costs (~0.41USD per analysis), but also reduces the resultant waste to the environment.

scholarly journals A simple spectrophotometric method for the determination of methyldopa using p-chloranil in the presence of hydrogen peroxide

2008 ◽  
Vol 33 (3) ◽  
pp. 7-12 ◽  
Author(s):  
M. A. Gotardo ◽  
L. S. Lima ◽  
R. Sequinel ◽  
J. L. Rufino ◽  
L. Pezza ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification ◽  
Coefficients Of Variation ◽  
The Common ◽  
Interday Precision ◽  
Sensitive Spectrophotometric Method

A simple, rapid and sensitive spectrophotometric method has been developed for the determination of methyldopa in pharmaceutical formulations. The method is based on the reaction between tetrachloro-p-benzoquinone (p-chloranil) and methyldopa, accelerated by hydrogen peroxide (H2O2), producing a violet-red compound (λmax = 535 nm) at ambient temperature (25.0 ± 0.2 ºC). Experimental design methodologies were used to optimize the measurement conditions. Beer's law is obeyed in a concentration range from 2.10 x 10-4 to 2.48 x 10-3 mol L-1 (r = 0.9997). The limit of detection was 7.55 x 10-6 mol L-1 and the limit of quantification was 2.52 x 10-5 mol L-1. The intraday precision and interday precision were studied for 10 replicate analyses of 1.59 x 10-3 mol L-1 methyldopa solution and the respective coefficients of variation were 0.7 and 1.1 %. The proposed method was successfully applied to the determination of methyldopa in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95 % confidence level.

Red-Excitation Dispersive Raman Spectroscopy is a Suitable Technique for Solid-State Analysis of Respirable Pharmaceutical Powders

2005 ◽  
Vol 59 (3) ◽  
pp. 286-292 ◽  
Author(s):  
Reinhard Vehring
Keyword(s):  
Raman Spectroscopy ◽  
Limit Of Detection ◽  
High Sensitivity ◽  
Instrument Design ◽  
Background Suppression ◽  
Pharmaceutical Powders ◽  
Limit Of Quantification ◽  
Mass Fractions ◽  
Suitable Technique ◽  
Spray Dried

Dispersive Raman spectroscopy with excitation by a red diode laser is suitable for quantitative crystallinity measurements in powders for pulmonary drug delivery. In spray-dried mixtures of salmon calcitonin and mannitol, all three crystalline polymorphs of mannitol and amorphous mannitol were unambiguously identified and their mass fractions were measured with a limit of quantification of about 5%. The instrument design offered high sensitivity and adequate background suppression, resulting in a low limit of detection in the range of 0.01% to 1%. This spectroscopy method has significant advantages over established techniques regarding specificity, sensitivity, and sample requirements.

scholarly journals Ultraviolet Spectrophotometric Method for Determination of Glipizide in Presence of Liposomal/Proliposomal Turbidity

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Neelkant Prasad ◽  
Roshan Issarani ◽  
Badri Prakash Nagori
Keyword(s):  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Clear Solution

A simple and sensitive ultraviolet spectrophotometric method for quantitative estimation of glipizide in presence of lipid turbidity is described to avoid false estimation due to diffraction by turbidity. UV detection was performed at 230 nm, 225 nm, and 235 nm, and the calibration curve was plotted between resultant of absorbance of [230 nm − (225 nm + 235 nm)/2] and concentration of analyte. The calibration curve was linear over the concentration range tested (1–20 μg/mL) with limit of detection of 0.27 μg/mL and limit of quantification of 0.82 μg/mL. Percent relative standard deviations and percent relative mean error, representing precision and accuracy, respectively, for clear as well as turbid solutions, were found to be within acceptable limits, that is, always less than 0.69 and 0.41, respectively, for clear solution and 0.65 and 0.47, respectively, for turbid solution. Conclusively, our method was successfully applied for the determination of glipizide in clear as well as turbid solutions, and it was found that the drug analyte in both types of solutions can be detected from the same calibration curve accurately and precisely and glipizide entrapped in the liposomes or in proliposomal matrix was not detected.

scholarly journals Pengembangan Biosensor Berbasis Plastik Zona Mikro untuk Skrining Aktivitas Antidiabetes pada Ekstrak Tanaman Obat

2021 ◽  
Vol 9 (1) ◽  
pp. 41
Author(s):  
Indri Firma Wati ◽  
Bambang Kuswandi ◽  
Dwi Koko Pratoko
Keyword(s):  
Diabetes Mellitus ◽  
Response Time ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Linear Range ◽  
T Test ◽  
Antidiabetic Activity ◽  
Limit Of Quantification ◽  
Antidiabetic Agents

Research on the diabetes mellitus (DM) treatment has recently been carried out, especially on discovering antidiabetic agents derived from plants. This study aims to determine the fabrication of microzone plastic-based biosensors, determine the optimal sensor conditions, analysis characteristics, and compare the biosensor with the UV-Vis spectrophotometric method. The results showed that the response time was 15 minutes, the linear range was 500-40000 µg / mL (R = 0.9989). The limit of detection (LOD) was 1109.6 µg / mL, and the limit of quantification (LOQ) was 3698.8 µg / mL. Biosensor filled up the precision parameters with an RSD value of less than 3.7% and an accuracy with recovery in the range of 95-105%. The biosensor is stable in storage at 25 ° C for 270 minutes and at chiller temperature for three days. The antidiabetic activity of the biosensor was compared with the UV-Vis spectrophotometer using the Independent Sample T-test and showed insignificant differences between the two methods.

scholarly journals Development and ICH Validation of a RP-HPLC-UV Method for the Quantification of Thimerosal in Topic Creams

2017 ◽  
Vol 60 (4) ◽  
Author(s):  
Guadalupe Pérez-Caballero ◽  
Nancy Muro-Hidalgo ◽  
Elvia Adriana Morales-Hipólito ◽  
Alma Villaseñor ◽  
Raquel López-Arellano
Keyword(s):  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Reversed Phase ◽  
Sample Treatment ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Quality Control Tool

A reversed phase high-performance liquid chromatography (RP-HPLC) method for determination of Thimerosal (TMS) in topical creams was optimized and validated according to the ICH guidelines which include accuracy, precision, selectivity, robustness, limit of detection (LOD), limit of quantification (LOQ), linearity and range. For topical creams, sample treatment is often an overwhelming step essentially due to its oily nature. For the first time a simple and robust extraction procedure for TMS using phosphate buffer (pH 5.5, 0.2M) was successfully developed. This method describes the TMS quantitation by HPLC in a topical product containing 0.01% fluocinolone acetonide (FLA) as the active molecule. The HPLC separation was achieved on a Column Symmetry® and a methanol: phosphate buffer (pH 2.5, 0.05M) 70:30 v/v mobile phase and wavelength 218 nm. Results from both standards and samples showed adequate validation parameters. Noteworthy, linearity was within the range 1.2 - 2.8 μg/mL. Additionally, robustness and TMS stability were established after sample extraction. The method provides an efficient and safe quality control tool for determination of TMS in topical creams.

Analytical Method Development and Validation of UV-visible Spectrophotometric Method for the Estimation of Vildagliptin in Gastric Medium

Drug Research ◽  
2020 ◽  
Vol 70 (09) ◽  
pp. 417-423
Author(s):  
Beena Kumari ◽  
Aparna Khansili
Keyword(s):  
Melting Point ◽  
Spectrophotometric Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Scanning Calorimetry ◽  
Limit Of Quantification ◽  
Double Beam ◽  
Uv Visible ◽  
Development And Validation

Abstract Background Vildagliptin is an antidiabetic agent, belongs to the dipeptidyl peptidase IV (DPP-4) inhibitors. Objective The aim of investigation was to develop a simple UV-visible Spectrophotometric method for the determination of vildagliptin in its pure form and pharmaceutical formulations, further to validate the developed method. Material and Methods Vildagliptin was estimated using UV-Visible double beam spectrophotometer at the wavelength of maximum absorption (210 nm) in acidic medium containing 0.1N HCl. The drug was characterized by melting point, Differential Scanning Calorimetry (DSC), and Fourier Transform Infra-Red (FTIR) techniques. The analysis of the drug was carried out by novel UV-Visible method which was validated analytical parameters like linearity, precision, and accuracy as per guidelines laid down by International Conference on Harmonization (ICH). Result Melting point of drug was found 154°C which is corresponds to its actual melting range. Similarly by the interpretation of spectra the drug was confirmed. The linear response for concentration range of 5–60 µg/ml of vildagliptin was recorded with regression coefficient 0.999. The accuracy was found between 98–101%. Precision for intraday and interday was found to be 1.263 and 1.162 respectively, which are within the limits. To establish the sensitivity of the method, limit of detection (LOD) and limit of quantification (LOQ) were determined which were found to be 0.951 µg/ml and 2.513 µg/ml respectively. Conclusion The UV method developed and validated for vildagliptin drug was found to be linear, accurate, precise and economical which can be used for the testing of its pharmaceutical formulations.

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