Determination of genotoxic impurities N-nitrosodimethylamine and N-nitrosodiethylamine in chondroitin sulfate sodium raw materials by liquid-liquid extraction/GC-MS
Objective:To establish a liquid-liquid extraction method for the determination of genotoxic impuri-ties N-nitrosodimethylamine(NDMA)and N-nitrosodiethylamine(NDEA)in chondroitin sulfate sodium by gas chromatography-mass spectrometry(GC-MS).Methods:The chromatographic column was Thermo TG WAXMS(30 m × 0.25 mm,0.25 µm).The column temperature was maintained at 40 ℃ for 1 min,increased to 240 ℃at 25 ℃·min-1 and maintained for 2 min.The inlet temperature was 220 ℃.The carrier gas was high-purity helium,and the flow rate was 1.0 mL·min-1.The ion source of mass spectrometry was EI source.The electron energy was 70 eV.The ion source temperature was 280 ℃ and the transmission line temperature was 240 ℃.Injection volume was 1 µL.Results:The LOD of NDMA was 0.64 ng·mL-1.Experiment showed a good linear relationship between peak area and concentration in the range of 4-16 ng·mL-1,and the correla-tion r was 0.999 3.The LOD of NDEA was 0.176 ng·mL-1 with a good linear relationship between peak area and concentration within the range of 1.1-4.4 ng·mL-1.The correlation r was 0.999 6.NDMA and NDEA were not detected in chondroitin sulfate sodium.Conclusion:The method is simple,specific and can be used to determine the genotoxic impurities NDMA and NDEA in chondroitin sulfate sodium.
gas chromatography-mass spectrometryliquid-liquid extractiongenotoxic impuritiesN-ni-trosodimethylamineN-nitrosodimethylaminechondroitin sulfate sodium
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