scholarly journals Quantitative Determination and Sampling of Lamivudine and Zidovudine Residues for Cleaning Validation in a Production Area

2007 ◽  
Vol 90 (3) ◽  
pp. 715-719 ◽  
Author(s):  
Maria InÊs Rocha Miritello Santoro ◽  
Tatiana Tatit Fazio ◽  
Anil Kumar Singh ◽  
Erica Rosa Maria Kedor-Hackmann
Keyword(s):  
Chromatography Method ◽  
Drug Products ◽  
Cleaning Validation ◽  
Relative Standard ◽  
Immunodeficiency Virus ◽  
Production Area ◽  
The Mean ◽  
Liquid Chromatography Method ◽  
Carry Over

Abstract Lamivudine (3TC) and zidovudine (AZT) are systemic antiviral substances extensively used in human immunodeficiency virus (HIV) infected patients. Nowadays, 3TC, AZT, and several other pharmacologically potent pharmaceuticals are manufactured in the same production area. To assure quality of drug products and patient safety, properly validated cleaning methodology is necessary. A carefully designed cleaning validation and its evaluation can ensure that residues of 3TC and AZT will not carry over and cross contaminate the subsequent product. The aim of this study was to validate a simple analytical method for verification of residual 3TC and AZT in equipment used in the production area and to confirm the efficiency of the cleaning procedure. The liquid chromatography method was validated using a Nova-Pak<sup/> C18 column (3.9 150 mm, 4 m particle size) and methanolwater (20 + 80, v/v) as the mobile phase at a flow rate of 1.0 mL/min. Ultraviolet detection was made at 266 nm. The calibration curve was linear over a concentration range of 2.022.0 g/mL with a correlation coefficient of 0.9998. The detection and quantitation limits were 0.36 and 1.21 g/mL, respectively. The intra-day and interday precision expressed as relative standard deviation were below 2.0%. The mean recovery of the method was 99.19%. The mean extraction recovery from manufacturing equipment was 83.5%.

scholarly journals HPLC Quantification of Cytotoxic Compounds fromAspergillus niger

2017 ◽  
Vol 2017 ◽  
pp. 1-7
Author(s):  
Paula Karina S. Uchoa ◽  
Leandro Bezerra de Lima ◽  
Antonia T. A. Pimenta ◽  
Maria da Conceição F. de Oliveira ◽  
Jair Mafezoli ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
High Performance ◽  
Chromatography Method ◽  
Relative Standard ◽  
Validation Parameters ◽  
Cytotoxic Compounds ◽  
Liquid Chromatography Method ◽  
Marine Strain

A high-performance liquid chromatography method was developed and validated for the quantification of the cytotoxic compounds produced by a marine strain ofAspergillus niger. The fungus was grown in malt peptone dextrose (MPD), potato dextrose yeast (PDY), and mannitol peptone yeast (MnPY) media during 7, 14, 21, and 28 days, and the natural products were identified by standard compounds. The validation parameters obtained were selectivity, linearity (coefficient of correlation > 0.99), precision (relative standard deviation below 5%), and accuracy (recovery > 96).

scholarly journals Compartmental Pharmacokinetics of the Antifungal Echinocandin Caspofungin (MK-0991) in Rabbits

2001 ◽  
Vol 45 (2) ◽  
pp. 596-600 ◽  
Author(s):  
Andreas H. Groll ◽  
Bryan M. Gullick ◽  
Ruta Petraitiene ◽  
Vidmantas Petraitis ◽  
Myrna Candelario ◽  
...  
Keyword(s):  
High Performance ◽  
Pharmacokinetic Model ◽  
Area Under The Curve ◽  
Apparent Volume ◽  
Volume Of Distribution ◽  
Pharmacokinetic Parameters ◽  
Chromatography Method ◽  
Opportunistic Fungi ◽  
The Mean ◽  
Liquid Chromatography Method

ABSTRACT The pharmacokinetics of the antifungal echinocandin-lipopeptide caspofungin (MK-0991) in plasma were studied in groups of three healthy rabbits after single and multiple daily intravenous administration of doses of 1, 3, and 6 mg/kg of body weight. Concentrations were measured by a validated high-performance liquid chromatography method and fitted into a three-compartment open pharmacokinetic model. Across the investigated dosage range, caspofungin displayed dose-independent pharmacokinetics. Following administration over 7 days, the mean peak concentration in plasma (C max) ± standard error of the mean increased from 16.01 ± 0.61 μg/ml at the 1-mg/kg dose to 105.52 ± 8.92 μg/ml at the 6-mg/kg dose; the mean area under the curve from 0 h to infinity rose from 13.15 ± 2.37 to 158.43 ± 15.58 μg · h/ml, respectively. The mean apparent volume of distribution at steady state (Vdss) was 0.299 ± 0.011 liter/kg at the 1-mg/kg dose and 0.351 ± 0.016 liter/kg at the 6-mg/kg dose (not significant [NS]). Clearance (CL) ranged from 0.086 ± 0.017 liter/kg/h at the 1-mg/kg dose to 0.043 ± 0.004 liter/kg/h at the 6-mg/kg dose (NS), and the mean terminal half-life was between 30 and 34 h (NS). Except for a trend towards an increasedVdss, there were no significant differences in pharmacokinetic parameters in comparison to those after single-dose administration. Caspofungin was well tolerated, displayed linear pharmacokinetics that fit into a three-compartment pharmacokinetic model, and achieved sustained concentrations in plasma that were multiple times in excess of reported MICs for susceptible opportunistic fungi.

scholarly journals Simple and Rapid Liquid Chromatography Method for Determination of Rifabutin in Plasma

2013 ◽  
Vol 9 (2) ◽  
pp. 26-29 ◽  
Author(s):  
AK Hemanth Kumar ◽  
V Sudha ◽  
Geetha Ramachandran
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

A high performance liquid chromatographic method for determination of rifabutin in human plasma was  developed. The method involved deproteinisation of the sample with acetonitrile and analysis of the  supernatant using a reversed-phase C18 column (250mm) and UV detection at a wavelength of 265nm.  The assay was specific for rifabutin and linear from 0.025 to 10.0μg/ml. The relative standard deviation  of intra- and inter-day assays was lower than 10%. The method was able to remove interfering materials  in plasma, yielding an average recovery of rifabutin from plasma of 101%. Due to its simplicity, the assay  can be used for pharmacokinetic studies of rifabutin. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS; 2012; IX(2) 26-29 DOI: http://dx.doi.org/10.3126/saarctb.v9i2.7975

scholarly journals Amphenicols stability in medicated feed – development and validation of liquid chromatography method

2014 ◽  
Vol 58 (4) ◽  
pp. 621-629 ◽  
Author(s):  
Wojciech Jerzy Pietro ◽  
Aneta Woźniak ◽  
Katarzyna Pasik ◽  
Wojciech Cybulski ◽  
Dorota Krasucka
Keyword(s):  
Liquid Chromatography ◽  
Analytical Procedure ◽  
Chromatography Method ◽  
The Matrix ◽  
The Mean ◽  
Liquid Chromatography Method ◽  
Sensitivity Specificity ◽  
Development And Validation ◽  
Feed Samples

Abstract A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF) and thiamphenicol (TAP) in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3) on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm) analytical column with UV (λ = 220 nm) detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.

scholarly journals PHARMACEUTICAL QUALITY ASSESSMENT OF GLIMEPIRIDE TABLETS – COMPARISON OF BRANDS AND NEWLY FORMULATED TABLETS WITH INNOVATOR

2021 ◽  
pp. 63-67
Author(s):  
SHAHNAZ USMAN ◽  
M. BASSAM ISMAIL SHEHADA ◽  
ANAB USMAN ◽  
QUAMRUL ISLAM
Keyword(s):  
Drug Release ◽  
High Performance ◽  
P Value ◽  
Drug Release Profile ◽  
Chromatography Method ◽  
Drug Products ◽  
Accuracy And Precision ◽  
Weibull Models ◽  
Kinetic Assessment ◽  
Liquid Chromatography Method

Objective: The main objective of the study was to assess the quality attribute of generic brands and newly formulated tablet of glimepiride and compare their drug release profile with innovator brand. Methods: Different brands were purchased from different markets of UAE. The validated high-performance liquid chromatography method was used to assess the quantitative analysis of glimepiride. The linearity of curve (r² = 0.9999) indicated the accuracy and precision of the analytical method. Comparative dissolution of newly formulated and generic tablets was carried out using USP dissolution apparatus II. Study was accomplished in phosphate buffer (pH = 7.8), the paddle speed was adjusted at 75 rpm. F1 and F2 factor among the brands and kinetic assessment were done to obtain the order of release. Results: Dissolution profiles of formulated tablets were almost same as that of innovator, 91.53 and 94.9, respectively, in 15 min. The statistical value between the different brands (F = 3.698) indicated that there were some differences among the few groups of tablets and p-value (0.002154) indicated that it supported H1 hypothesis. First-order and Weibull models described the drug release with r2 value of 0.9981–0.927210 and 0.9992– 0.9835, respectively. Stability of optimized formulated batch was also examined. Conclusion: It was concluded that the formulated tablets are stable and pharmaceutically as good as the innovators; however, all the selected brands could not be used interchangeably in the clinical practice. It was also concluded that the scrutiny and screening of the drug products, available in the markets, can help to build a better health-care setup.

scholarly journals A novel method of reversed migration capillary electrophoresis for determination of linear alkylbenzene sulfonates

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Zhuo Huang ◽  
Weike Wang ◽  
Lingxian Xie ◽  
Li Lin
Keyword(s):  
Capillary Electrophoresis ◽  
High Performance ◽  
Ph Value ◽  
High Sensitivity ◽  
Chromatography Method ◽  
Linear Alkylbenzene ◽  
Relative Standard ◽  
Linear Alkylbenzene Sulfonates ◽  
Liquid Chromatography Method ◽  
And Migration

AbstractA reversed migration capillary electrophoresis (RMCE) has been developed to determine linear alkylbenzene sulfonates (LAS). The sample stacking and separation conditions have been systematically investigated and optimized under reversed separation voltage at a low pH value. The separation effect of LAS homologs has been greatly improved based on the relative motion of electrophoresis and electroosmotic flow. RMCE demonstrates a good linear range of 0.1 mg/l to 10.0 mg/l, and the detection limit of LAS homologs reaches 0.001–0.004 mg/l. The relative standard deviations (n=6) of peak area and migration time were 2.25–4.40% and 0.67–0.75%, respectively. RMCE has also been applied for LAS detection in practical wastewater. The results show RMCE exhibits easy pretreatment, fast detection, high sensitivity, good peak shapes and resolution, and less solvent consumption, compared with the established high-performance liquid chromatography method.

scholarly journals A Broadly Accessible Liquid Chromatography Method for Quantification of Six Nitrosamine Compounds and N,N-Dimethylformamide in Metformin Drug Products Using High Resolution Mass Spectrometry

2020 ◽  
Author(s):  
Qian Wu ◽  
Evgenia Kvitko ◽  
Nicola Zenzola ◽  
Kaury Kucera ◽  
David Light
Keyword(s):  
High Resolution Mass Spectrometry ◽  
The United States ◽  
High Mass ◽  
Chromatography Method ◽  
Drug Products ◽  
Regulatory Guidance ◽  
High Mass Resolution ◽  
United States Food ◽  
States Food ◽  
Liquid Chromatography Method

N-nitrosodimethylamine (NDMA) and the industrial solvent, N,N-dimethylformamide (DMF), are both probable human carcinogens that have been detected in pharmaceutical drug products like metformin, which is used to treat type II diabetes. Some lots of metformin drug products have exceeded the United States Food and Drug Administration (FDA) daily allowable intake limit for NDMA, while the presence of DMF has been detected at several orders of magnitude higher than NDMA. A recent study found that a low abundance isotope of DMF interferes with NDMA quantification by using a unique subset of LC-MS instruments capable of high mass resolution. In this study, an LC-HRMS method is developed that chromatographically separates NDMA from DMF in metformin drug products to eliminate interference. The method can detect nitrosamines and DMF under the current regulatory guidance for industry and provides a solution for simultaneously quantifying nitrosamines and DMF for a broad range of LC-MS instruments.

scholarly journals Development, Validation, and Routine Application of a High-Performance Liquid Chromatography Method Coupled with a Single Mass Detector for Quantification of Itraconazole, Voriconazole, and Posaconazole in Human Plasma

2010 ◽  
Vol 54 (8) ◽  
pp. 3408-3413 ◽  
Author(s):  
Lorena Baietto ◽  
Antonio D'Avolio ◽  
Giusi Ventimiglia ◽  
Francesco Giuseppe De Rosa ◽  
Marco Siccardi ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Internal Standard ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
True Value ◽  
Relative Standard ◽  
Mass Detector ◽  
Liquid Chromatography Method

ABSTRACT We have developed and validated a high-performance liquid chromatography method coupled with a mass detector to quantify itraconazole, voriconazole, and posaconazole using quinoxaline as the internal standard. The method involves protein precipitation with acetonitrile. Mean accuracy (percent deviation from the true value) and precision (relative standard deviation percentage) were less than 15%. Mean recovery was more than 80% for all drugs quantified. The lower limit of quantification was 0.031 μg/ml for itraconazole and posaconazole and 0.039 μg/ml for voriconazole. The calibration range tested was from 0.031 to 8 μg/ml for itraconazole and posaconazole and from 0.039 to 10 μg/ml for voriconazole.

scholarly journals A fully validated microbiological assay to evaluate the potency of ceftriaxone sodium

2013 ◽  
Vol 49 (4) ◽  
pp. 753-762 ◽  
Author(s):  
Maria Luisa Manfio ◽  
Danielle Araújo Agarrayua ◽  
Jaison Carlosso Machado ◽  
Cleber Alberto Schmidt
Keyword(s):  
Low Cost ◽  
Pharmaceutical Formulations ◽  
Microbiological Assay ◽  
Intermediate Precision ◽  
Chromatography Method ◽  
Beta Lactamases ◽  
Pharmaceutical Samples ◽  
Ceftriaxone Sodium ◽  
Relative Standard ◽  
Liquid Chromatography Method

Ceftriaxone (CFTX) sodium is a third-generation, broad-spectrum cephalosporin that is resistant to beta-lactamases. An alternative bioassay for the assessment of the potency of this drug in pharmaceutical formulations has not been previously reported. Thus, this paper reports the development and full validation of a 3 x 3 agar diffusion bioassay using a cylinder-plate method to quantify CFTX sodium in pharmaceutical samples. The strain Staphylococcus aureus ATCC 6538P was used as the test microorganism, and the results of the proposed bioassay displayed high linearity, precision, accuracy, specificity and robustness. All potency results were statistically analyzed using an analysis of variance (ANOVA) and were found to be linear (r=0.99999) in the range of 16-64 µg/mL, accurate (100.5%), and precise [repeatability: relative standard deviation (RSD)=1.4%; intermediate precision: between-day RSD=2.1% and between-analyst RSD=2.5%]. The specificity of the bioassay was determined by evaluating a degraded sample (50 ºC) at 0, 24 and 48 hours as compared against the results from the pharmacopeial liquid chromatography method for CFTX. The results validated the proposed microbiological assay, which allows reliable quantitation of CFTX in pharmaceutical samples. Moreover, it is a useful, simple and low-cost alternative method for monitoring the quality of this medicine.

Sign in / Sign up

Export Citation Format

Share Document