Objective To establish a gas-mass spectrometry method for determination of epichlorohydrin in Metoprolol succinate tablets.Methods The chromatographic column is HP-1MS.Injection temperature is 220℃;The injection method is split injection,and the split ratio is 10:1.The heating procedure is to keep the initial temperature at 50℃ for 3 min,then raise the temperature to 80℃at a rate of 20℃/min for 5 min,and to 280℃at a rate of 40℃/min for 8 min.The sample intake capacity is 1 μL.The ion source is electron bombardment source(EI),ion source temperature is 230℃.Mass spectrometry interface temperature is 260℃;the monitoring mode of mass spectrometry is SIM.The mass to charge ratios(m/z)are 49,57 and 62.Results The linear range of epichlorohydrin concentration is 30～120 ng/mL(r>0.99).The detection limit is 32.37 ng/mL.The limit of quantitation is 107.89 ng/mL.RSD of precision is 1.8％(n=6).The average recovery is 103.8％with RSD of 2.5％(n=6).Epichlorohydrin was not detected in 3 batches of Metoprolol succinate tablets.Conclusion The established gas-mass coupling method is simple,practical,accurate and reliable,and can be used for the determination of epichlorohydrin in Metoprolol succinate tablets.
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