Simultaneous determination of four nitrosamine impurities in the raw material of ademetionine 1,4-butanedisulfonate by gas chromatography-triple quadrupole mass spectrometry
Simultaneous determination of four nitrosamine impurities in the raw material of ademetionine 1,4-butanedisulfonate by gas chromatography-triple quadrupole mass spectrometry
A method for simultaneous determination of four nitrosamine genotoxic impurities in the raw material of ademetionine 1,4-butanedisulfonate by gas chromatography-triple quadrupole mass spectrometry was established.After the sample was dissolved in water and extracted with dichloromethane as the extractant,it was separated using VF-624 ms capillary column(30 m×0.25 mm,1.4 µm)and quantitatively detected using the standard curve method.The inlet temperature wss 220℃,the carrier gas was high-purity helium,and the flow rate was 1.0 mL/min,with sample injection volume of 1 μL.The ion source was EI source,and the temperature of that was 250℃.The mass concentration of four types of nitrosamine impurities had a good linear relationship with the corresponding quantitative ion response values in the range of 0.24-20.84 ng/mL,and the correlation coefficients were all more than 0.99.The detection limits of the method were 0.12-0.52 ng/mL,and the quantification limits were 0.24-1.04 ng/mL.The average recoveries of sample spiked were 80.7%-102.4%,and the relative standard deviations of the determination results were 5.3%-7.3%(n=9).This method can be used for the determination of nitrosamine impurities in ademetionine 1,4-butanedisulfonate,providing a reference for its quality control.
关键词
气相色谱-三重四级杆质谱法/丁二磺酸腺苷甲硫氨酸/亚硝胺杂质
Key words
gas chromatography-triple quadrupole mass spectrometry/ademetionine 1,4-butanedisulfonate/nitrosamine impurities
维普
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