scholarly journals Development and Validation of Optical Methods for Zeta Potential Determination of Silica and Polystyrene Particles in Aqueous Suspensions

Materials ◽  
2021 ◽  
Vol 14 (2) ◽  
pp. 290
Author(s):  
Yannic Ramaye ◽  
Marta Dabrio ◽  
Gert Roebben ◽  
Vikram Kestens
Keyword(s):  
Zeta Potential ◽  
Particle Tracking ◽  
Colloidal Stability ◽  
Optical Methods ◽  
Intermediate Precision ◽  
Electrophoretic Light Scattering ◽  
Measurement Uncertainties ◽  
Development And Validation ◽  
Direct Implementation

Zeta potential is frequently used to examine the colloidal stability of particles and macromolecules in liquids. Recently, it has been suggested that zeta potential can also play an important role for grouping and read-across of nanoforms in a regulatory context. Although the measurement of zeta potential is well established, only little information is reported on key metrological principles such as validation and measurement uncertainties. This contribution presents the results of an in-house validation of the commonly used electrophoretic light scattering (ELS) and the relatively new particle tracking analysis (PTA) methods. The performance characteristics were assessed by analyzing silica and polystyrene reference materials. The ELS and PTA methods are robust and have particle mass working ranges of 0.003 mg/kg to 30 g/kg and 0.03 mg/kg to 1.5 mg/kg, respectively. Despite different measurement principles, both methods exhibit similar uncertainties for repeatability (2%), intermediate precision (3%) and trueness (4%). These results confirm that the developed methods can accurately measure the zeta potential of silica and polystyrene particles and can be transferred to other laboratories that analyze similar types of samples. If direct implementation is impossible, the elaborated methodologies may serve as a guide to help laboratories validating their own methods.

scholarly journals Development and Validation of a Green Analytical Method for the Determination of Aspirin and Domperidone Bulk or Formulation Using UV and HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 49-56
Author(s):  
Sneha Jagnade ◽  
Pushpendra Soni ◽  
Lavakesh Kumar Omray
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Research Work ◽  
Ultra Violet ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation

The aim of present study was to investigate the development and validation of a green analytical method for the determination of aspirin and domperidone. Method Development and Validation for Estimation of Domperidone and Aspirin in bulk or formulation by using RP-HPLC. The RP-HPLC method was developed for estimation of Aspirin and Domperidone in synthetic mixture by isocratically using 10 mM KH2PO4: Acetonitrile (20:80) as mobile phase, Prontosil C-18 column (4.6 x 250 mm, 5μparticle size) column as stationary phase and chromatogram was recorded at 231 nm. Then developed method was validated by using various parameters such as, linearity, Range accuracy, precision repeatability, intermediate precision, robustness, limit of detection, limit of quantification. The proposed methods were found to be linear with correlation coefficient close to one. Precision was determined by repeatability, Intermediate precision and reproducibility of the drugs. The robustness of developed method was checked by changing in the deliberate variation in solvent. The result obtained shows the developed methods to be Cost effective, Rapid (Short retention time), Simple, Accurate (the value of SD and % RSD less than 2), Precise and can be successfully employed in the routine analysis of these drugs in bulk drug as well as in tablet dosage form. The Simplicity, Rapidly and Reproducibility of the proposed method completely fulfill the objective of this research work. Keywords: Asprin; Domperidone; HPLC; Ultra Violet; Validation

scholarly journals DEVELOPMENT AND VALIDATION OF A TLC DENSITOMETRIC METHOD FOR DETERMINATION OF GLIMEPIRIDE IN TABLETS

2014 ◽  
Vol 16 (1) ◽  
pp. 11-15
Author(s):  
Yuni Retnaningtyas ◽  
Lestyo Wulandiri ◽  
Gabriella F Punu
Keyword(s):  
Pharmaceutical Analysis ◽  
Data Recovery ◽  
Antidiabetic Drug ◽  
Intermediate Precision ◽  
Quantification Limit ◽  
Accuracy And Precision ◽  
Quality Control Testing ◽  
The Mean ◽  
Development And Validation

A simple and valid TLC method has been developed for the determination of glimepiride in tablet formulation. After extraction of the analyte with a mixture of methanol and ammonia 0,2M (1:1, v/v), the extracts were spotted on precoated TLC silica gel F254 plates, which were developed with a mixture of toluene:methanol:ethyl acetate (75:20:5, v/v/v). Quantitative evaluation was performed by measuring the absorbance reflectance of the analyte spots at 238 nm. The method was validated for specificity, linearity, accuracy and precision. Good linearity was achieved in the concentration range 100–800 ng/spot. The RSD of repeatability and intermediate precision were found to be less than 2%, whereas the mean of the recovery data was 100-101%. The detection limit and quantification limit were 22 and 74 ng/spot, respectively. The method is specific, linear, precise, and accurate; it can be used for the routine quality control testing of marketed formulations.Keywords: glimepiride, TLC densitometric, validation of pharmaceutical methods, pharmaceutical analysis, antidiabetic drug Sebuah metode Kromatografi Lapis Tipis (KLT) yang sederhana dan valid telah dikembangkan untuk penentuan glimepiride dalam sediaan tablet. Setelah analit dalam sampel diekstraksi dengan campuran metanol dan amonia 0,2 M (1:1,v/v), ekstrak yang terlihat pada lempeng silika gel F254, yang dikembangkan dengan campuran toluen : metanol : etil asetat (75:20:5, v/v/v). Evaluasi kuantitatif dilakukan dengan mengukur reflektansi absorbansi noda analit pada panjang gelombang 238 nm.Metode ini divalidasi meliputi spesifisitas, linearitas, akurasi dan presisi.Linearitas yang baik dicapai pada rentang konsentrasi 100-800 ng / spot. RSD pengulangan dan presisi intermediate menunjukkan nilai kurang dari 2 %, sedangkan rata-rata data recovery adalah 100-101 % .Batas deteksi dan batas kuantifikasi adalah 22 dan 74 ng / noda.Metode ini spesifik, linear, tepat, dan akurat, bisa digunakan untuk pengujian kontrol kualitas rutin tablet glimepirid dipasarkan. Kata Kunci: glimepiride, TLC densitometric, validation of pharmaceutical methods, pharmaceutical analysis, antidiabetic drug

scholarly journals Development and Validation of RP-LC Method for the Determination of Cinnarizine/Piracetam and Cinnarizine/Heptaminol Acefyllinate in Presence of Cinnarizine Reported Degradation Products

2013 ◽  
Vol 8 ◽  
pp. ACI.S12478 ◽  
Author(s):  
Ola M. EL-Houssini ◽  
Nagwan H. Zawilla ◽  
Mohammad A. Mohammad
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Good Resolution ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Reverse Phase Liquid Chromatography ◽  
Phase Liquid ◽  
Development And Validation

Specific stability indicating reverse-phase liquid chromatography (RP-LC) assay method (SIAM) was developed for the determination of cinnarizine (Cinn)/piracetam (Pira) and cinnarizine (Cinn)/heptaminol acefyllinate (Hept) in the presence of the reported degradation products of Cinn. A C18 column and gradient mobile phase was applied for good resolution of all peaks. The detection was achieved at 210 nm and 254 nm for Cinn/Pira and Cinn/Hept, respectively. The responses were linear over concentration ranges of 20-200, 20-1000 and 25-1000 μgmL−1 for Cinn, Pira, and Hept respectively. The proposed method was validated for linearity, accuracy, repeatability, intermediate precision, and robustness via statistical analysis of the data. The method was shown to be precise, accurate, reproducible, sensitive, and selective for the analysis of Cinn/Pira and Cinn/Hept in laboratory prepared mixtures and in pharmaceutical formulations.

DEVELOPMENT AND VALIDATION OF THE PROCEDURE FOR QUANTITATIVE DETERMINATION OF IMPURITIES IN TABLETS “RANOLAZIN-NAN”

2021 ◽  
Vol 92 (2) ◽  
pp. 80-92
Author(s):  
V. B. Klimashevich ◽  
E. V. Kokusev ◽  
V. V. Gudovich ◽  
O. A. Kazyuchits ◽  
A. I. Zhebentyaev
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Intermediate Precision ◽  
Column Temperature ◽  
Related Impurities ◽  
Stability Robustness ◽  
Quantitation Limit ◽  
The Stability ◽  
Development And Validation

The article presents the results of the research on the development of the procedure for determining related impurities by high-performance reversed-phase chromatography in the tablets “Ranolazin-NAN”. The conditions for samples preparation of ranolazine tablets, optimal conditions for the gradient mode of chromatography were selected using Zorbax Eclipse Plus C18 column: eluent A - 0,1% triethylamine buffer with pH 6,0 ± 0,1 (diluted with orthophosphoric acid) and acetonitrile in a ratio 70:30 v / v and eluent B - acetonitrile. The effect of pH medium (2,0, 6,0 and 9,0) on the efficiency of the column while studying the solutions of ranolazine and identified impurities was established. The suitability of the chromatographic system was proven and the specificity of the method for determining unidentified and identified impurities was proven. Linearity in the entire range of the procedure usage (from the quantitation limit to 125% (of the content of a single impurity)), correctness as well as precision at the level of reproductivity and intermediate precision, and the stability (robustness) of the method with small changes in the flow rate and column temperature were proven for the procedure of related impurities determination in Ranolazin-NAN tablets.

scholarly journals Development and Validation of an Agar Diffusion Assay for Determination of Ceftazidime in Pharmaceutical Preparations

2008 ◽  
Vol 91 (1) ◽  
pp. 59-66 ◽  
Author(s):  
Cleber A Schmidt ◽  
Marcelly Carazzo ◽  
Luciane V Laporta ◽  
Celso F Bittencourt ◽  
Marcos R Santos ◽  
...  
Keyword(s):  
Pharmaceutical Preparations ◽  
Inhibitory Effect ◽  
Intermediate Precision ◽  
Agar Diffusion ◽  
Test Microorganism ◽  
Relative Standard ◽  
Alternative Methodology ◽  
Development And Validation ◽  
Liquid Chromatographic

Abstract Ceftazidime (CFZ) is a broad spectrum parenterallactam antibiotic of the cephalosporin family. This paper reports the development and validation of an agar diffusion microbiological assay using the cylinder-plate method for determination of CFZ in powder for injection. The validation carried out yielded good results in terms of linearity, precision, accuracy, selectivity, and robustness. The assay is based on the inhibitory effect of CFZ upon the strain of Pseudomonas aeruginosa ATCC 27853 used as the test microorganism. The results of the assays were treated statistically by analysis of variance and were found to be linear (correlation coefficient = 0.999998) in the selected range of 8.032.0 g/mL; precise [repeatability: relative standard deviation (RSD) = 1.11; intermediate precision: between-day RSD = 1.37 and between-analyst RSD = 1.41]; and accurate. The selectivity of the bioassay was evaluated by analysis of degraded samples at 50C, and the results were compared with a pharmacopeial liquid chromatographic method at the time 0, 24, and 48 h. The results demonstrated the validity of the proposed bioassay, which allows reliable quantitation of CFZ in pharmaceutical samples and can be used as a useful alternative methodology for CFZ analysis in routine quality control.

scholarly journals Development and Validation of GC-ECD Method for the Determination of Metamitron in Soil

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Shishir Tandon ◽  
Satyendra Kumar ◽  
N. K. Sand
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Retention Time ◽  
Intermediate Precision ◽  
Pesticide Monitoring ◽  
Precision And Accuracy ◽  
Development And Validation ◽  
Sensitive Method ◽  
Detection And Quantification

This paper aims at developing and validating a convenient, rapid, and sensitive method for estimation of metamitron from soil samples.Determination andquantification was carried out by Gas Chromatography on microcapillary column with an Electron Capture Detector source. The compound was extracted from soil using methanol and cleanup by C-18 SPE. After optimization, the method was validated by evaluating the analytical curves, linearity, limits of detection, and quantification, precision (repeatability and intermediate precision), and accuracy (recovery). Recovery values ranged from 89 to 93.5% within 0.05- 2.0 µg L−1with average RSD 1.80%. The precision (repeatability) ranged from 1.7034 to 1.9144% and intermediate precision from 1.5685 to 2.1323%. Retention time was 6.3 minutes, and minimum detectable and quantifiable limits were 0.02 ng mL−1and 0.05 ng g−1, respectively. Good linearity (R2=0.998) of the calibration curves was obtained over the range from 0.05 to 2.0 µg L−1. Results indicated that the developed method is rapid and easy to perform, making it applicable for analysis in large pesticide monitoring programmes.

scholarly journals DEVELOPMENT AND VALIDATION OF AN RP-HPLC METHOD FOR THE DETERMINATION OF ULIPRISTAL ACETATE IN BULK AND PHARMACEUTICAL DOSAGE FORM

2021 ◽  
pp. 83-89
Author(s):  
SANATHOIBA SINGHA S ◽  
SREENIVAS RAO T
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Ulipristal Acetate ◽  
Relative Standard ◽  
Development And Validation

Objective: This work makes an attempt to establish a sensitive and accurate method for the development and validation of an analytical method for estimation of ulipristal acetate (UPA) in bulk and pharmaceutical dosage form. Methods: A mixture of 20 mM acetate buffer pH 3.7 and methanol in the ratio of 70:30 (v/v %) was used as the mobile phase. An xBridge™ C18 column (250 mm × 4.6 mm, 5μ) was used for the analysis at a flow rate of 1 ml/min, injection volume of 20 μl, run time of 15 min, and detection wavelength of 309 nm. The repeatability (within-day in triplicates) and intermediate precision (for 2 days) were carried out by six injections and the obtained results within and between the days of trials were expressed as percent relative standard deviation (% RSD). The linearity of the method was determined by the analysis of analyte concentration across a range of 10 μg/ml–60 μg/ml. Results: The % RSD values of precision studies were found to be below the accepted limit of 2%. The method was found to be linear with a correlation coefficient (R2) of 0.98. The method was also found to be accurate and robust with suitable values. Limit of detection (LOD) and limit of quantification (LOQ) of the method were found to be 0.371 μg/ml and 1.23 μg/ml, respectively. Conclusion: The results of analysis prove that this method can be used for the routine determination of UPA in bulk drug and in pharmaceutical dosage forms.

scholarly journals Development and validation of an LC-MS/MS method for the determination of adapalene in pharmaceutical forms for skin application

2016 ◽  
Vol 81 (10) ◽  
pp. 1171-1181 ◽  
Author(s):  
Vladimir Dobricic ◽  
Natasa Bubic-Pajic ◽  
Bojan Markovic ◽  
Sote Vladimirov ◽  
Snezana Savic ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Intermediate Precision ◽  
Column Temperature ◽  
Mobile Phases ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Chromatographic Parameters ◽  
Development And Validation

Development and validation of a liquid chromatography - tandem mass spectrometry (LC-MS/MS) method for the determination of adapalene in pharmaceutical forms for skin application were presented. The MS/MS analysis of adapalene was performed by use of three mobile phases, consisted of acetonitrile and (a) 0.1 % formic acid, (b) 0.1 % trifluoroacetic acid and (c) 20 mM ammonium acetate. The strongest signals of parent ion and dominant product ion were obtained in negative mode by use of the mobile phase (c). Validation of this method was performed according to the ICH guidelines. Small variations of selected chromatographic parameters (concentration of ammonium acetate, mobile phase composition, column temperature and flow rate) did not affect qualitative and quantitative system responses significantly, which proved method?s robustness. The method is specific for the determination of adapalene. Linearity was proved in the concentration range 6.7 - 700.0 ng mL-1 (r = 0.9990), with limits of detection and quantification 2.0 ng mL-1 and 6.7 ng mL-1, respectively. Accuracy was confirmed by calculated recoveries (98.4 % - 101.5 %). Precision was tested at three levels: injection repeatability, analysis repeatability and intermediate precision. Calculated relative standard deviations were less than 1, 2 and 3 %, respectively.

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