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Determination of N ‐Nitrosodimethylamine and N ‐Nitrosodiethylamine in Sartans and Metformin Raw Materials and Finished Products by Headspace Gas Chromatography‐Tandem Mass Spectrometry
Author(s) -
Lim HyunHee,
Oh YunSuk,
Shin HoSang
Publication year - 2020
Publication title -
bulletin of the korean chemical society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.237
H-Index - 59
ISSN - 1229-5949
DOI - 10.1002/bkcs.12085
Subject(s) - chemistry , chromatography , isotope dilution , mass spectrometry , gas chromatography , gas chromatography/tandem mass spectrometry , gas chromatography–mass spectrometry , electrospray ionization , detection limit , n nitrosodimethylamine , tandem mass spectrometry , analytical chemistry (journal) , organic chemistry , carcinogen
A simple and sensitive headspace (HS) and gas chromatography‐isotope dilution tandem mass spectrometric method was studied to determine N ‐nitrosodimethylamine (NDMA) and N ‐nitrosodiethylamine (NDEA) in sartans and metformin raw materials and their finished products. The HS parameters were optimized and selected. Samples in headspace vial were extracted at 150°C for 15 min and analyzed by injecting 1.0 mL of the headspace into the gas chromatography–mass spectrometry (GC–MS)/MS system. The mass spectrometer was operated using the electrospray ionization and detection was performed in a multiple reaction monitoring mode. Under the established condition, the lower limits of detection was 0.4 μg/kg for NDMA and 0.1 μg/kg for NDEA by using 0.1 g of sample. The precision was in the range of 0.4–3.5% for NDMA, and 0.4–3.3% for NDEA, and the accuracy was in the range of 95.0–105% for NDMA and 93.6–103% for NDEA, respectively. The linear equation of the calibration curve is y = 0.0120 x − 0.0202 (4.0–1080 μg/kg, r = 1.000) for NDMA, and y = 0.0144 x − 0.0042 (0.5–288 μg/kg, r = 1.000) for NDEA. The developed method can be applied to all six sartans and one metformin raw materials and their finished products.