High Pressure Liquid Chromatographic Method for the Determination of Mobocertinib in Pharmaceutical Dosage Form and Study of Its Degradation

Aims: New validated method for the estimation of Mobocertinib using HPLC and study of its degradation. Place and Duration of Study: Department of Chemistry, RVR & JC College of Engineering, Chowdavaram, Guntur, Andhra Pradesh, between February 2021 and August 2021. Methodology: Using an X-bridge phenyl column (150 mm x 4.6 mm, 3.5 µ), acetonitrile, and 0.1 percent ortho phosphoric acid (OPA) (60:40 v/v) as a mobile phase, the proposed method successfully achieved effective chromatographic separation with a flow rate of 1 mL/min and a wave length of 224 nm. Mobocertinib had a retention time of 2.271 minutes. The isocratic chromatography was performed at room temperature and took approximately five minutes to complete. Results: Analysis was achieved within 5 min over an honest linearity within the concentration range from 6-90 µg/ml of Mobocertinib. Using a mathematical process, the suitability parameters of the system were investigated, and the results were found to be in acceptable limits. In a linear analysis, stages with regression coefficients of 0.999 were used. LOD and LOQ values were 0.075μg/ml and 0.248 g/ml for Mobocertinib. The drug was recovered at a rate of 98-102 percent, which means that the recovery is within reasonable limits. Conclusion: The validation results were satisfactory, and the approach was found to be suitable for bulk and formulation analysis. The recommended procedure was found to be warranted according to ICH guidelines.

Stability Demonstrating Validated High Pressure Liquid Chromatographic Method for the Determination of Trilaciclib in Bulk and Pharmaceutical Formulation

Aims: New validated method for the estimation of Trilaciclib using HPLC and study of its degradation Place and Duration of Study: Department of Chemistry, RVR & JC College of Engineering, Chowdavaram, Guntur, Andhra Pradesh, between February 2021 and August 2021. Methodology: Using an inertsil ODS column (150 mm x 4.6 mm, 3.5 µ), acetonitrile, and 0.1 percent ortho phosphoric acid (OPA) (50:50 v/v) as a mobile phase, the proposed method successfully achieved effective chromatographic separation with a flow rate of 1 mL/min and a wave length of 220 nm. Trilaciclib had a retention time of 4.358 minutes. The isocratic chromatography was performed at room temperature and took approximately six minutes to complete. Results: Analysis was achieved within 6 min over an honest linearity within the concentration range from 3-45 µg/ml of Trilaciclib. Using a mathematical process, the suitability parameters of the system were investigated, and the results were found to be in acceptable limits. In a linear analysis, stages with regression coefficients of 0.999 were used. LOD and LOQ values were 0.038 μg/ml and 0.124 g/ml for trilaciclib. The drug was recovered at a rate of 98-102 percent, which means that the recovery is within reasonable limits. Conclusion: The validation results were satisfactory, and the approach was found to be suitable for bulk and formulation analysis. The recommended procedure was found to be warranted according to ICH guidelines.

An Ultra-High-Pressure Liquid Chromatographic Tandem Mass Spectrometry Method for the Analysis of Benzoyl Ester Derivatized Glycols and Glycerol.

Presented is an ultra-high-pressure liquid chromatographic tandem mass spectrometry (UPLC–MS/MS) method developed for the detection of propylene glycol, glycerol, ethylene glycol and diethylene glycol using isotopically labeled standards in urine as part of ongoing studies to evaluate whether urinary propylene glycol and/or vegetable glycerin concentration are indicators of recent use. Propylene glycol and vegetable glycerol are found in many products that are consumed and used including electronic cigarettes (e-cigarettes). E-cigarettes are battery-powered devices used as an alternative to traditional cigarettes. The liquid formulations aerosolized in these devices largely consist of propylene glycol and/or vegetable glycerol. Published reports regarding the ratio of propylene glycol to glycerol content in these formulations ranged from 50:50 to 100 percent of either. For the analysis of urine specimens from both users and non-users of e-cigarettes, calibrators, controls and specimens were derivatized using benzoyl chloride prior to analysis. They were analyzed using a Waters AcQuity Xevo TQ-S Micro UPLC–MS/MS. Chromatographic separation was performed on an AcQuity UPLC BEH C18 1.7 um, 2.1 × 50 mm, column using a 20 mM ammonium formate in water and 20 mM ammonium formate in methanol as the mobile phase. The method was validated using SWGTOX guidelines for linearity, precision and accuracy, stability, carryover and limit of detection. The linear range was determined using a seven-point calibration curve ranging between 0.5 and 100 mcg/mL. The bias for all validation controls was determined to be ±20% of the expected concentrations with CVs of <15%. A total of 124 urine specimens analyzed collected with 50 specimens collected from self-reported non-smokers (cigarettes/e-cigarettes) confirmed cotinine free using the DRI® Cotinine Assay (Thermo Scientific, Waltham, MA) and 74 specimens collected before and after 12 hours self-reported e-cigarettes abstinence e-cigarette users. Propylene glycol and glycerol were determined to have concentration ranges of “none detected” to 1470 and “none detected” to 2950 mcg/mL, respectively.

ENANTIOSELECTIVE ANALYSIS OF GUAIFENESIN IN BULK AND PHARMACEUTICAL DOSAGE FORMS BY CHIRAL REVERSE PHASE HPLC-PDA METHOD

A novel, accurate and precise chiral reverse-phase high pressure liquid chromatographic method was developed for enantioselective analysis of guaifenesin (GFN) in bulk and tablet dosage forms. Chiral separation was achieved on phenomenex Lux Cellulose-4 column (250×4.6mm, 5μ) using 0.02% formic acid: acetonitrile (90:10 V/V) as the mobile phase at a flow rate of 1mL/min at 230nm. The retention times of GFN enantiomers A and B was 15 and 16 minutes, respectively, with good peak resolutions and showing good linearity in the concentration range of 10-50 μg/mL (R2 > 0.999). The developed method was validated as per the International Conference on Harmonization guidelines and the results were well within the acceptable limits. The percentage assay in tablet dosage form was found to be 98.8 and 98.2 respectively, for enantiomers A and B and was with in the compendial specifications, demonstrating the suitability of developed method for enantioselective analysis of guaifenesin racemic mixture.

Fast gradient normal-phase high pressure liquid chromatography for rapid baseline separation of vitamin E forms in palm-derived tocotrienol rich fractions (TRFs)

A normal phase high pressure liquid chromatographic method was developed for the simultaneous determination of nine vitamin E forms comprised of α-tocomonoenol, α-, β-, γ-, and δ-tocopherols and α-, β-, γ-, and δ-tocotrienols in tocotrienol rich fractions (TRFs) derived from palm oil.