Determination of MBT in cefazoxime sodium for injection by UPLC-MS-MS and risk analysis of domestic samples
Objective:To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS)method for the determination of 2-mercaptobenzothiazole(MBT)genotoxic impurities in cefazoxime sodium for injection and to analyze the detection of domestic samples from 28 manufacturers.Methods:The UPLC analysis was performed on a Phenomenex Luna Omega C18 column,(2.1 mm × 100 mm,1.6 μm)with the column temperature 30 ℃.The mobile phases A was 2 mmol·L-1 ammonium acetate(contai-ning 0.001％formic acid)and the mobile phase B was acetonitrile with gradient elute.The flow rate was 0.3 mL·min-1.The injection volume was 5 µL.The electrospray ionization(ESI)source in positive mode and multiple reaction monitoring(MRM)were used for the detection of MBT,and external standard method for quanti-tative analysis.Results:The linear relationship of MBT was good in the concentration range of 1.4-58.12 ng·mL-1(r=0.999).The limit of detection was 1.453 pg and the limit of quantification was 7.265 pg.The average recoveries of low,medium and high concentrations were 106.8％,107.1％and 109.0％,respectively with the relative standard deviation(RSD)all less than 2.0％.The relative standard deviation(RSD)of repeatability was less than 6.0％.The content of MBT in the samples from 28 domestic enterprises was all less than 10 ppm,but there were obvious differences in the detected amount among all enterprises which is due to different production processes.Conclusion:The established method can be used for the qualitative and quantitative detection of MBT in cefazoxime sodium for injection and the partical enterprises which have been detected MBT impurities need to further raise the warning.
万方数据
维普
