Lee, Do Hee Hwang, Su Hyeon Park, Seoungchul Lee, Jeongmi Oh, Han Bin Han, Sang Beom Liu, Kwang-Hyun Lee, Yong-Moon Pyo, Hee Soo Hong, Jongki 2024-01-19T14:02:18Z 2024-01-19T14:02:18Z 2021-10-21 2021-08-14 1759-9660 https://pubs.kist.re.kr/handle/201004/116588 A solvent-free headspace gas chromatography-mass spectrometry (SF-HS-GC/MS) method was developed and validated for screening N-nitrosodimethylamine (NDMA) in various active pharmaceutical ingredients (APIs) and drug products. Experimental parameters such as incubation temperature, incubation time, and sample volume in solvent-free headspace conditions were optimized. The developed SF-HS-GC/MS method was validated in terms of linearity, limit of quantification (LOQ), precision, and accuracy. The results indicated excellent linearity from 5 to 500 ng g(-1) with correlation coefficients higher than 0.9999. The LOQ of this method was 5 ng g(-1) and matrix effects ranged from 0.97 to 1.11. The accuracy ranged from 92.77 to 106.54% and the precision RSDs were below 5.94%. No significant matrix effect was observed for any of the drug products. Also, artefactual NDMA formation in ranitidine, nizatidine, and metformin was investigated under HS conditions. Adjusted (mild) SF-HS conditions were suggested for precise quantification of NDMA in positive drug products by GC/MS. The present SF-HS-GC/MS method is a promising tool for the screening and determination of toxic NDMA in APIs and drug products. English ROYAL SOC CHEMISTRY PERFORMANCE LIQUID-CHROMATOGRAPHY NITROSAMINES A solvent-free headspace GC/MS method for sensitive screening of N-nitrosodimethylamine in drug products Article 10.1039/d1ay01036k 1 ANALYTICAL METHODS, v.13, no.30, pp.3402 - 3409 ANALYTICAL METHODS 13 30 3402 3409 scie scopus 000671928200001 2-s2.0-85112182055 Chemistry, Analytical Food Science & Technology Spectroscopy Chemistry Food Science & Technology Spectroscopy Article PERFORMANCE LIQUID-CHROMATOGRAPHY NITROSAMINES