Aug 2026· Rapid Communications in Mass Spectrometry· Vol 40 20, pp.
e70157
· 0 citations· 32 references
Medicine
TL;DR
This study provided a reference method for the quality control of NVCM hydrochloride using UHPLC-QTOF-MS and elucidated the chemical structures of the impurities.
Abstract
Rationale
Norvancomycin (NVCM) hydrochloride belongs to a group of glycopeptide antibiotics and exhibits strong effects against Gram-positive cocci and bacilli. The safety of patients' lives is directly related to the quality of drugs. The impurities play often an important role in this process. This study aimed to investigate the impurity profile of NVCM hydrochloride.
Methods
To identify the impurities, a simple and sensitive ultrahigh performance liquid chromatography quadrupole-time-of-flight mass spectrometry (UHPLC-QTOF-MS) method was developed. An ACQUITY UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) was used. The flow rate was set at 0.2 mL/min. Mobile phase (A) consisted of 10 mmol/L ammonium formate (pH 9.0) and mobile phase (B) was methanol. Gradient elution was performed as follows: 0-5 min, 15% B; 5-25 min, 15% B to 20% B; 25-40 min, 20% B to 70% B. Stress degradation experiments were conducted to check the specificity of the method.
Results
Thirteen impurities and two degradation products were characterized using UHPLC-QTOF-MS.
Conclusions
Based on MS/MS spectral data and exact mass measurements, the chemical structures of the impurities were elucidated. This study provided a reference method for the quality control of NVCM hydrochloride.
A robust LC-MS method is established for the separation and quantification of Dimethylglyoxime foreign substancein Lenalidomide. Chromatographic separation was accomplished using a Zorbax Eclipse C18, 100 X4.6 mm, 3.5µcolumn. A Mixture of 0.01M of Ammonium formate as 50v/v and Acetonitrile as 50 v/v used as the mobile phase. The rate of flow is measured at 0.40mL/min with Gradient elution and mass spectrometry operating in positive ionmode. Selectivity of the method proved that protonated species of Dimethylglyoxime (m/z 117.16) separatedfromLenalidomid drug substances, with a exceptional linearity over a range of 6-120 ppm, limits of detection of 2.00ppm and quantification of 6.05 ppm. Consistent recovery rates were obtained between 90-100%, and the analytical
solution remained stable for up to 72 hours at 2-8ºC. Subsequently, the developed and validated analytical methodwas assessed for environmental sustainability using established greenness assessment tools. The AGREEscore wascalculated at 0.62, and the BAGI value at 70.0. These values reflected a favorable environmental profile, efficient
sample preparation, and practical sustainability. These proposed separation strategies showed high specificity, substantiating clear resolution of DMG foreign substance by the drug compound, also with foreign substances. Together, these metrics confirmed the method’s suitability for both regulatory compliance and routine applicationinindustrial Quality Control laboratories.
M. Srinivas, B. Andrews, V. D. N. Kumar Abbaraju et al.· RASAYAN Journal of Chemistry· 0 citations
Valbenazine tosylate is a drug indicated for the management of tardive dyskinesia. This study presents the optimization of chromatographic methods to assess the inherent stability of this molecule. The stability studies were executed as per the ICH guidelines, integrating multiple stress conditions that involved hydrolytic conditions with pH variation, oxidative, photolytic, and thermal degradation. An HPTLC system from CAMAG was used, utilizing silica gel 60 F254 plates. The mobile phase was a mixture of toluene and methanol in a 7:3 volume ratio. Detector was set at 280 nm. An HPLC system included a pump (PU 2080 Plus) and PDA detector (MD 2010 Plus). Acetonitrile and acetate buffer pH 5 were used as the optimized phase. ICH Q2 (R1) guideline was referred to validate the optimized methods. Forced degradation studies indicated that valbenazine was susceptible to alkaline hydrolytic conditions, and was relatively stable under the other stress conditions.
M. Damle, Dipti S. Bhorade· Indian drugs· 0 citations
Background: Bedaquiline, a diarylquinoline inhibitor of ATP synthase is an important drug in the treatment of multidrug resistant tuberculosis (MDR TB) but due to its lipophilic property and low plasma levels, sensitive measurement of this drug is difficult. Method: To achieve the first UPLC assay for bedaquiline in human plasma, the method was developed and is now completely validated based on ICH guidelines. The separation was carried out on a Thermo Hypurity C18 column using acetonitrile–ammonium acetate (60:40, v/v) as the mobile phase with bedaquiline d6 as the internal standard. Results and Discussion: The method achieved excellent linearity with r2 of 0.999, over the range of 25-225 µg/mL, accuracy of 94-110% and precision of < 7%CV. Different types of plasma (lipemic, hemolyzed etc.) all had a recovery of around 70%. Freeze–thaw, bench-top exposure and storage of processed samples did not cause a loss of stability. Using a simple precipitation clean up and UPLC. Using the Lean Six Sigma (DMAIC) concept, the workflow was methodically optimized for efficiency, reproducibility and compliance to regulations. Conclusion: This assay appears to be an alternative and the procedure provides a quick, selective and reproducible method for pharmacokinetic study and therapeutic drug monitoring where TB patients are infected with MDR TB than previous HPLC methods.
K. N. Maneesha, B. R. Kuber· Genetics and Molecular Resea...· 0 citations
This study presents the development and validation of analytical methods for the quantitative estimation of Esomeprazole, the S-enantiomer of omeprazole and a potent proton pump inhibitor (PPI) widely used in the management of acid-related gastrointestinal disorders including GERD, peptic ulcer disease, and Zollinger–Ellison syndrome. Two complementary analytical techniques – UV spectrophotometry and RP-HPLC – were developed and validated in accordance with ICH guidelines. The UV method involved measuring the absorbance of Esomeprazole at 305 nm using methanol as solvent. The method demonstrated excellent linearity within the concentration range of 2–12 µg/mL, with a correlation coefficient (r²) of 0.9961. The RP-HPLC method was optimized using a mobile phase of 0.1% Triethylamine: Methanol (70:30, v/v), with detection at 250 nm on a C18 column (250 × 4.6 mm, 5 µm) at a flow rate of 1.0 mL/min, yielding a retention time of approximately 4.13 minutes. The HPLC method demonstrated linearity over the concentration range of 32–48 µg/mL (80–120%), with a correlation coefficient (r²) of 0.9998. Validation parameters including precision, accuracy, LOD, LOQ, specificity, repeatability, and robustness confirmed the suitability of both methods. Both analytical methods were found to be simple, precise, accurate, economical, and reproducible, confirming their applicability for routine quality control of Esomeprazole in pharmaceutical dosage forms.
A. K, Mahesh Kumar S, S. T· Genetics and Molecular Resea...· 0 citations
Objectives Mavacamten (MYK-461), approved for hypertrophic cardiomyopathy, is a cardiac myosin inhibitor. At present, no pharmacopoeial method for its quantification has been reported. Our study was designed to establish a validated stability-indicating reverse-phase high-performance liquid chromatography method to quantify MYK-461 in its capsule formulation. Materials and Methods For chromatographic separation, an Inertsil ODS-3V C18 column (250 × 4.6 mm, 5 µm) with the mobile phase of 0.1% trifluoroacetic acid and acetonitrile (50:50 v/v) was used. The flow rate (1.0 mL/min), column temperature (35 °C), injection volume (10 µL), total run time (10 minutes), and detection wavelength (269 nm) were applied. Results The validated method showed precision, accuracy, and robustness, with relative standard deviation < 2% and recovery of 100.5%. Linearity was observed over the range 5–75 µg/mL (r = 0.9994). We achieved a clear, well-resolved separation of MYK-461 from impurities, with estimated limit of detection (1.58 µg/mL) and limit of quantification (4.8 µg/mL). In forced degradation studies, we observed the highest degradation under acidic conditions (10.37%), while minimal degradation under photolytic (0.93%), thermal (1.66 %), oxidative (2.56%), and alkaline (4.19%) conditions. Conclusion The developed method is precise and reliable, and offers a practical tool for routine quality control and future research, while emphasising the need for controlled storage conditions to ensure long-term drug integrity.
P. Daroi, Pranjali Patil, V. Munipalli et al.· Turkish Journal of Pharmaceu...· 0 citations
Cystic fibrosis, a genetic disorder caused by mutations in the CFTR gene, is commonly treated using combination therapy with IVA and LUMA. Accurate quantification of these drugs in human plasma is essential for therapeutic monitoring; however, conventional analytical methods often lack sufficient sensitivity and robustness. In this study, a QbD-based RP-UPLC method was developed and validated for the simultaneous estimation of IVA and LUMA in human plasma. The primary objective was to achieve efficient separation of analytes from plasma interferences with reduced run time and consistent analytical performance. Chromatographic separation was carried out using a Waters Acquity UPLC system equipped with a CSH C18 column (100 mm × 2.1 mm, 1.8 μm). Method optimization was performed using a Central Composite Design model. The mobile phase is 0.01 N ammonium acetate and acetonitrile (60:40, v/v) at a flow rate of 0.3 mL/min, with the column maintained at 30°C. EMT was used as the internal standard, and detection was conducted at 260 nm. The retention times were 1.45, 1.77, and 1.99 min for EMT, IVA, and LUMA, respectively. The method is reliable, rapid and selective, exhibiting excellent linearity, precision, and accuracy, complying with USFDA guidelines.
Subbarao Jhampani, Rayini Venkata Sai Mounica, S. Vidhyadhara· Biomedical chromotography· 0 citations
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