Trace-level quantification of NDMA in levosulpuride active pharmaceutical ingredient and tablet formulation Using UFLC-MS/MS
Hemanth Vikram P․R,
Gunjan Kumar,
Rajashree Deka,
Umme Hani,
Nazima Haider,
Sirajunisa Talath,
Adil Farooq Wali,
Dilipkumar Reddy Kandula,
Narasimha M. Beeraka,
Sinchana B Gopalaiah,
Devi Sri Chiriki,
Namitha Bannimath,
Pramod Kumar,
Bannimath Gurupadayya
Affiliations
Hemanth Vikram P․R
Department of Pharmaceutical Chemistry, JSS College of Pharmacy Mysuru, JSS Academy of Higher Education and Research (JSSAHER), Mysuru, 570015, India; Xenone Healthcare Pvt. Ltd., New Delhi, 110076, India
Gunjan Kumar
Xenone Healthcare Pvt. Ltd., New Delhi, 110076, India
Rajashree Deka
Department of Zoology, Bhattadev University, Bajali, Pathsala, 781325, Assam, India
Umme Hani
Department of Pharmaceutics, College of Pharmacy, King Khalid University, Abha 62529, Saudi Arabia
Nazima Haider
Department of Pathology, College of Medicine, King Khalid University, Abha 62529, Saudi Arabia
Sirajunisa Talath
Department of Pharmaceutical Chemistry, RAK College of Pharmacy, RAK Medical and Health Sciences University, Ras Al Khaimah 11172, United Arab Emirates
Adil Farooq Wali
Department of Pharmaceutical Chemistry, RAK College of Pharmacy, RAK Medical and Health Sciences University, Ras Al Khaimah, United Arab Emirates
Dilipkumar Reddy Kandula
Department of Pharmacy, Shri Jagdishprasad Jhabarmal Tibrewala University, Jhunjhunu, 333010, Rajasthan, India
Narasimha M. Beeraka
Department of Human Anatomy and Histology, I.M. Sechenov First Moscow State Medical University (Sechenov University), Moscow, 119991, Russia; Department of Pharmacology, Raghavendra Institute of Pharmaceutical Education and Research (RIPER), Ananthapuramu, 515721, India; Herman B. Wells Center for Pediatric Research, Department of Pediatrics, Indiana University School of Medicine, Indianapolis, 46202, USA; Department of Studies in Molecular Biology, University of Mysore, Mysore, Karnataka 570006, India
Sinchana B Gopalaiah
Department of Pharmaceutical Analysis, SRM College of Pharmacy, SRM Institute of Science and Technology, Kattankulathur, India
Devi Sri Chiriki
Department of Pharmaceutical Chemistry, JSS College of Pharmacy Mysuru, JSS Academy of Higher Education and Research (JSSAHER), Mysuru, 570015, India
Namitha Bannimath
Department of Pharmacology, University of Galway, University Road, Galway, H91 TK33, Ireland
Pramod Kumar
Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research (NIPER)-Guwahati, Changsari, 781101, India
Bannimath Gurupadayya
Department of Pharmaceutical Chemistry, JSS College of Pharmacy Mysuru, JSS Academy of Higher Education and Research (JSSAHER), Mysuru, 570015, India; Corresponding author.
Nitrosamine impurities identified in several pharmaceuticals during recent times has raised concerns leading to product recalls worldwide and necessitating sensitive liquid and gas chromatographic methods for trace level detection of nitrosamine impurities. This study developed and validated a ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) method for the quantification of NDMA in Levosulpuride drug substance and tablet formulation. Current method utilizes a triple quadrupole analyzer, atmospheric pressure chemical ionization (APCI) ionization source and multiple reaction monitoring (MRM) scan mode for the analysis. Chromatographic separation was achieved on a Gemini NX-C18 column (150 × 4.6 mm, 3 µm) maintained at 40 °C. The mobile phase consisted of a binary gradient of solvent A (0.1 % formic acid in water) and solvent B (methanol), with a total run time of 18 minutes. Current method achieved excellent linearity, recovery, precision, and sensitivity. Greenness of the developed method was evaluated using the GAPI, AGREE, and AES metrics. Current method is sensitive and selective for NDMA in levosulpuride drug substance and tablet formulations and can be employed for routine quality control analysis in pharmaceutical industry.
