Some colourants are hazardous to living organisms. Hence, a powerful and fast methodology is required for the analysis of those colourants in food and water samples. A modest electrochemically polymerised glutamic acid layered multi-walled carbon nanotube paste electrode [P(GA)LMWCNTPE] was functionalised for the sensing of indigo carmine (IC) by the differential pulse voltammetry (DPV) and cyclic voltammetry (CV) approaches. Within the optimised experimental conditions, the P(GA)LMWCNTPE holds an acceptable and high rate of electro-catalytic activity towards the redox behaviour of IC. The projected P(GA)LMWCNTPE shows a decent selectivity for IC in the presence of methyl orange. The modified sensor shows an acceptable linear growth between oxidative peak current and concentration in both CV and DPV methods with fine limit of detection values of 4.2 lM and 0.36 lM, respectively. Additionally, the developed sensor was effectively applied to detect IC in food and water samples. The morphological and surface activities of the modified and unmodified electrodes were determined through field emission scanning electron microscopy, electrochemical impedance spectroscopy, and CV techniques. The P(GA)LMWCNTPE requires a simple preparation procedure and is low-cost, with acceptable storage stability, sensitivity, and reproducibility.
A selective and sensitive novel methods were developed and validated for identification and trace level quantification (0.5 ppm) of genotoxic impurities Methyl 3‐amino‐4‐methylbenzoate, 3‐amino‐4‐methylbenzoic acid, and 3‐(4‐methyl‐1H‐imidazol‐1‐yl)‐5‐(trifluoromethyl) aniline in Nilotinib dihydrochloride active pharmaceutical ingredient by using liquid chromatography‐tandem mass spectrometry. The developed and validated methods were more accurate and capable to confirm the m/z values of parent and fragment ions through mass spectrometry and tandem mass spectrometry for further fragmentation. In addition, the developed methods were validated through current regulatory guidelines with a lower detection level of 0.15 ppm and a quantification level of 0.5 ppm for all the three genotoxic impurities. The correlation coefficient was observed as 0.9997 for Methyl 3‐amino‐4‐methylbenzoate genotoxic impurity‐I, 0.9998 for 3‐amino‐4‐methylbenzoic acid, and > 0.9999 for 3‐(4‐methyl‐1H‐imidazol‐1‐yl)‐5‐(trifluoromethyl) aniline. The recovery percentage of all the three genotoxic impurities was found to be between 93% to 105%.
A novel reversed-phase liquid chromatography coupled with tandem mass spectrometric (LC-MS/MS) method was developed and validated for the trace analysis of ethyl 2-amino-4,5-bis(2-methoxyethoxy)benzoate (ERL ethyl ester) and ethyl 4,5-bis(2-methoxyethoxy)-2-nitrobenzoate (ERL nitro compound) genotoxic impurities in Erlotinib Hydrochloride drug substance with the shorter run time. ERL ethyl ester and ERL nitro compound were identified as genotoxic impurities through DEREK nexus software. The method utilizes purosphere star RP 18 e (100 mm X 4.6 mm, 3.0 µm) column with electro spray ionization in multiple reaction monitoring (MRM) detection mode. The isocratic mode of elution for the impurities was carried out with the aid of the mobile phase using 0.1% formic acid in water & acetonitrile in the ratio of 42:58 v/v. The flow rate was 1.0 mL/min, column oven temperature 25ºC and elution was monitored by mass spectrometer. The method was validated as per International Conference on Harmonization (ICH) guidelines and quantitate up to 1 ppm of ERL ethyl ester and ERL nitro compound.
Objective: To develop and validate a selective, sensitive, rapid and accurate method using LC-MS/MS technique to achieve efficient separation between active pharmaceutical ingredient (Atazanavir sulphate) and genotoxic impurity (BOC epoxide).
Methods:The quantification was carried out using the column puro sphere star RP 18 e (length 150 mm, internal diameter 4.6 mm, particle size 3.0 µm) with electrospray ionization in multiple reaction monitoring (MRM) detection mode. Eluent-A was 0.1% formic acid in water and eluent-B was 0.1% formic acid and 0.1% ammonium hydroxide solution (25%) in acetonitrile. The isocratic mode of elution was carried out for the elution of impurity with the shorter run time of 6 min. The flow rate was 1.0 ml/min and column oven temperature was maintained 25 °C.
Results:The method was validated as per ICH guidelines and arrived the limit of detection and limit of quantification for the potential genotoxic impurity and found to be 0.2 ppm and 0.5 ppm. The developed method was found linear in the concentration range of 0.5 ppm to 6 ppm and accuracy results were within the range.
Conclusion:The developed short span method found to be selective, sensitive, precise and accurate for the quantification of the BOC epoxide genotoxic impurity in atazanavir sulphate drug substance.
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