Development and Validation of Genotoxic Impurity in Esomeprazole Magnesium Trihydrate Active Pharmaceutical Ingredient by LC-MS/MS

2019 ◽  
Vol 53 (4s) ◽  
pp. s642-s649
Author(s):  
Suresh Reddy Yelampalli ◽  
Venkata Shanmukha Kumar Jagarlapudi ◽  
Useni Reddy Mallu
Keyword(s):  
Active Pharmaceutical Ingredient ◽  
Esomeprazole Magnesium ◽  
Development And Validation

scholarly journals Development and Validation of 2-Azaspiro [4,5] Decan-3-One (Impurity A) in Gabapentin Determination Method Using qNMR Spectroscopy

Molecules ◽  
2021 ◽  
Vol 26 (6) ◽  
pp. 1656
Author(s):  
Nataliya E. Kuz’mina ◽  
Sergey V. Moiseev ◽  
Mikhail D. Khorolskiy ◽  
Anna I. Lutceva
Keyword(s):  
Test Procedure ◽  
Active Pharmaceutical Ingredient ◽  
Test Methods ◽  
Intermediate Precision ◽  
Coefficients Of Variation ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Student’S T ◽  
Development And Validation ◽  
Student’S T Test

The authors developed a 1H qNMR test procedure for identification and quantification of impurity A present in gabapentin active pharmaceutical ingredient (API) and gabapentin products. The validation studies helped to determine the limit of quantitation and assess linearity, accuracy, repeatability, intermediate precision, specificity, and robustness of the procedure. Spike-and-recovery assays were used to calculate standard deviations, coefficients of variation, confidence intervals, bias, Fisher’s F test, and Student’s t-test for assay results. The obtained statistical values satisfy the acceptance criteria for the validation parameters. The authors compared the results of impurity A quantification in gabapentin APIs and capsules by using the 1H qNMR and HPLC test methods.

scholarly journals Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Td Dft ◽  
High Level ◽  
Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

scholarly journals Validation of analytical method for determination of furosemide in extemporaneous syrup

2017 ◽  
Author(s):  
D. Alfred-Ugbenbo ◽  
O. A. Zdoryk ◽  
V. A. Georgiyants
Keyword(s):  
Sodium Hydroxide Solution ◽  
Correlation Coefficients ◽  
Active Pharmaceutical Ingredient ◽  
Stability Study ◽  
Assay Method ◽  
Pure Substance ◽  
Ultraviolet Region ◽  
Validation Parameters ◽  
Development And Validation ◽  
Medicinal Drugs

Introduction. Extreme syrups can be manufactured using substances or ready medicinal drugs as the active pharmaceutical ingredient. There is a necessity in the development and validation of analytical methods that can be used for quality control of pharmaceutical manufacturing of syrups containing furosemide.The aim of the study – to develop and validate assay method for furosemide in extemporaneous syrups prepared from both pure substance and finished products. Methods of the research. For proposed UV spectrophotometric assay method the conditions of analysis, sample preparation and validation characteristics were defined. Suspensions of substance and crushed commercial tablets were dissolved in 0.1 M sodium hydroxide solution and evaluated spectrophotometrically in ultraviolet region of light at a wavelength 271 nm using method of specific absorbance.Results and Discussion. Samples comply with the Beer-Lambert Bouguer law within the concentration range of 8×10-3 – 1.2×10-2 mg/ml with correlation coefficients ≥ 0.9981. The uncertainty of the methods was well within the critical value of the error (0.72 %≤ maxΔAs) for both samples of syrup containing pure substance and commercial tablets. Recovery studies for furosemide in syrup samples of substance and crushed commercial tablets yielded 99.92 ±0.54 % and 99.14±0.16 % respectively. Assay limit of ±10 % by the validation parameters: specificity, linearity, precision, accuracy within the range of 80–120 % of the nominal contents was met by all compounded preparations.Conclusions. The results of validation proved that this method can be reproduced correctly and is suitable for use in pharmaceutical analysis. Adoption of this method is planned in evaluating uniformity of content and, in combination of other methods, ascertain chemical stability study of compounded furosemide syrups.

Development and Validation of a Fast Stability-Indicating Ion-Paired Reversed-Phase HPLC Method for the Assay of Thiabendazole and Estimation of Its Related Compounds

2017 ◽  
Vol 100 (1) ◽  
pp. 74-81
Author(s):  
Peng Zhang ◽  
Jingzhi Tian ◽  
Abu Rustum
Keyword(s):  
Fruits And Vegetables ◽  
Methanesulfonic Acid ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Acid Sodium Salt ◽  
The Stability ◽  
Development And Validation ◽  
Related Compounds

Abstract Thiabendazole is a benzimidazole-based anthelmintic active pharmaceutical ingredient for the treatment of intestinal pinworm and Strongyloides infections. Thiabendazole is also used as a fungicide to control fungal diseases in fruits and vegetables. In this paper, we report, for the first time, the development and validation of a novel stability-indicating reversed-phase ion-paired HPLC method for the assay of thiabendazole and estimation of its related compounds. Chromatographic separation was achieved by using an isocraticelution at a flow rate of 1.5 mL/min using an ACE 5 C18 (4.6 × 50 mm, 5 μm particle size) columnmaintained at 35°C and with UV detection at 300 nm. The mobile phase consisted of 25% acetonitrile and75% 10 mM 1-octanesulfonic acid sodium salt aqueous solution containing 0.1% methanesulfonic acid. The total run time was only 4 min. The new method was successfully validated according to the International Conference on Harmonization guidelines. The stability-indicating capability of the method was demonstrated through adequate separation of all potential related compounds (from thiabendazole and from each other) present in aged and stressed degraded samples. The ion-paired HPLC method described in this paper is ideal for QC laboratories to conduct routine testing.

scholarly journals Development and Validation of a Method for the Semi-Quantitative Determination of N-Nitrosamines in Active Pharmaceutical Ingredient Enalapril Maleate by Means of Derivatisation and Detection by HPLC with Fluorimetric Detector

2021 ◽  
Vol 11 (16) ◽  
pp. 7590
Author(s):  
Dariusz Boczar ◽  
Elżbieta Wyszomirska ◽  
Beata Zabrzewska ◽  
Anna Chyła ◽  
Katarzyna Michalska
Keyword(s):  
Maximum Level ◽  
Active Pharmaceutical Ingredient ◽  
Test Sample ◽  
Hplc Method ◽  
Dansyl Chloride ◽  
Limit Of Quantification ◽  
Enalapril Maleate ◽  
Development And Validation ◽  
Blank Solution

A novel HPLC method with fluorimetric detection was developed for the determination of potentially carcinogenic N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) in active pharmaceutical ingredient enalapril maleate. N-nitrosamines were subject to denitrosation followed by derivatisation with dansyl chloride or fluorenylmethoxycarbonyl chloride (Fmoc-Cl). Fmoc-Cl offers much better sensitivity and repeatability than dansyl chloride derivatisation. A satisfactory linearity was obtained for the method, with R2 = 0.9994 for NDMA and 0.9990 for NDEA, and a limit of quantification level of 0.038 μg/g for NDMA and 0.050 μg/g for NDEA. The precision decreased with the concentration to a maximum level of about 10%. The recoveries were in the range of 74.2 ± 4.2% to 101.6 ± 16.1% for NDMA and 90.6 ± 2.9% to 125.4 ± 7.4% for NDEA. Dansyl chloride was found to be an inappropriate derivatisation agent, mainly due to potential contamination with dimethylamine, leading to unrepeatable peaks in the blank solution. Since the method involves the derivatisation of amines liberated from the N-nitrosamines, it was necessary to remove the amines from the test sample. Several critical points in the standard/sample preparation have been mentioned, which affect the reproducibility of the method and are not covered in similar articles.

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