Objective: To establish an HPLC-QQQ-MS/MS method for the determination of N-nitrosodimethylamine in ranitidine hydrochloride and nizatidine. Methods: The drugs were separated by a Phenomenex ACE Excel 3 C18-AR column（4.6 mm×100 mm,3 mm）with the mobile phases of 0.1% formic acid-water and 0.1% formic acid-methanol in gradient elution. The flow rate was 0.5 mL·min-1 and the column temperature was 40 ℃ . The detection wavelength of ranitidine hydrochloride and nizatidine was 230 nm and the injection volume was 5 μL. The atmospheric pressure chemical ionization source with positive ion mode was used for analyzing drugs in the multiple reaction monitoring mode. The transitions of m/z 75.0 → 43.0 and m/z 75.0 → 58.0 were applied as quantitative and qualitative ions respectively. Results: The linearity range of N-nitrosodimethylamine was 1-100 ng·mL-1;and the detection limit was 0.2 ng·mL-1. The contents of N-nitrosodimethylamine in 20 batches were 0.03-0.32 μg·g-1. Conclusion: This method can be used for the quantitation of N-nitrosodimethylamine in ranitidine hydrochloride and nizatidine.
YU Ying-jie, HUANG Hai-wei, ZHANG Long-hao, HU Nan, ZHANG Qing-sheng, HE Lan
. Determination of N-nitrosodimethylamine in ranitidine hydrochloride and nizatidine by HPLC-QQQ-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(6)
: 1019
-1023
.
DOI: 10.16155/j.0254-1793.2021.06.11
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