An orthogonal approach for method development and validation of three potential halo alkyl alcohol genotoxic impurities in miglitol drug substance by fast gas chromatography–mass spectrometry

2020 ◽  
Vol 3 (10) ◽  
pp. 511-522
Author(s):  
Nagaraju Rajana ◽  
D.V. Ramana ◽  
Rama Rao Ganta ◽  
Dharamasoth Rama Devi ◽  
Amol A. Deshpande ◽  
...  
Author(s):  
Jayavarapu Kumar Raja ◽  
Sundararajan Parimala Krishnan ◽  
Vankayala Devendiran Sundar

A new simple and precise Gas Chromatography Mass Spectrometry (GC-MS) method was developed and validated for the quantification of sonidegib in capsule formulation. The proposed work is depends on the modification of sonidegib into its derivative with N, O-bis(trimethylsilyl)-trifluoracetamide (BSTFA) with 1% trimethylchlorsilane (TMCS). Selective ion monitoring technique and electron ionization method at 70 eV were utilized for the quantification of sonidegib at m/z 278. Calibration plot was rectilinear in the concentration range of 0.5–10.0 µg/ml. The RSD value for within-day precision was ≤2.47% and for between-day precision was ≤2.45%. The bias value for within-day and between day accuracy was found between -1.51 to 1.87. The intra and inter day recovery findings of sonidegib was found to be between 98.34 to 102.654% for pharmaceutical formulation. The limits of detection and quantification of sonidegib were 0.10 and 0.30µg/ml respectively. No interfering peaks were observed from the excipients of dosage form during the analysis of formulation. The developed procedure was successfully applied for the quantification of commercial sonidegib capsule dosage form to estimate the sonidegib and to check the dosage form uniformity of content.


2020 ◽  
Vol 16 (8) ◽  
pp. 989-1019
Author(s):  
Habibur Rahman ◽  
S.K. Manirul Haque ◽  
Masoom Raza Siddiqui

Background: Schizophrenia is a severe mental illness that affects more than twenty-one million people throughout the world. Schizophrenia also causes early death. Schizophrenia and other related psychotic ailments are controlled by the prescription of antipsychotic drugs, which act by blocking certain chemical receptors in the brain and thus relieves the symptoms of psychotic disorder. These drugs are present in the different dosage forms in the market and provided in a certain amount as per the need of the patients. Objective: Since such medications treat mental disorders, it is very important to have a perfect and accurate dose so that the risk factor is not affected by a higher or lower dose, which is not sufficient for the treatment. For accurate assay of these kinds of drugs, different analytical methods were developed ranging from older spectrophotometric techniques to latest hyphenated methods. Results: The current review highlights the role of different analytical techniques that were employed in the determination and identification of antipsychotic drugs and their metabolites. Techniques such as spectrophotometry, fluorimetry, liquid chromatography, liquid chromatography-mass spectrometry, gas chromatography, and gas chromatography-mass spectrometry employed in the method development of such antipsychotic drugs were reported in the review. Different metabolites, identified using the hyphenated techniques, were also mentioned in the review. The synthesis pathways of few of the metabolites were mentioned. Conclusion: The review summarizes the analyses of different antipsychotic drugs and their metabolites. A brief introduction of illnesses and their symptoms and possible medications were highlighted. Synthesis pathways of the associated metabolites were also mentioned.


2004 ◽  
Vol 1035 (2) ◽  
pp. 237-247 ◽  
Author(s):  
Luigi Mondello ◽  
Alessandro Casilli ◽  
Peter Quinto Tranchida ◽  
Rosaria Costa ◽  
Biagina Chiofalo ◽  
...  

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