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建立了超高效液相色谱-串联质谱(UPLC-MS/MS)测定双氧水工作液中降解物的分析方法。样品用乙腈溶解后,采用ACCHROM C18(150 mm×4.6 mm,5μm)色谱柱,0.1%甲酸水溶液-乙腈为流动相体系,梯度洗脱,流速0.3 m L/min,柱温30℃,紫外检测波长254 nm;质谱采用电离子喷雾正离子模式检测。结果表明,双氧水工作液中有4种明显的降解物,采用面积归一法计算该4种降解物含量占降解物总量的80%以上;其它一些含量较低的降解物也能定性分析出。实验还采用了气相色谱-串联质谱法(GC-MS/MS)分析双氧水工作液,两种分析方法的结果能相互印证和互补,表明用色谱-串联质谱法能准确、全面地测定双氧水工作液中降解物,能为蒽醌法生产双氧水的企业对工作液中降解物的抑制和脱除提供参考。
A method for the determination of degradation products in hydrogen peroxide solution by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) was established. After the sample was dissolved in acetonitrile, the mobile phase was eluted with ACCHROM C18 (150 mm × 4.6 mm, 5 μm) column and 0.1% formic acid in water as mobile phase. The flow rate was 0.3 m L / min and the column temperature was 30 ℃. Wavelength 254 nm; Mass spectrometry ion-spray positive mode detection. The results showed that there were 4 obvious degradation products in the working solution of hydrogen peroxide solution, and the area degradation of the 4 degradation products accounted for more than 80% of the total degradation products by area normalization method. Other lower degradation products could also be qualitatively analyzed . The experiment also used gas chromatography-tandem mass spectrometry (GC-MS / MS) analysis of hydrogen peroxide working solution, the results of the two analysis methods can confirm each other and complement each other, indicating that chromatography - tandem mass spectrometry can accurately and completely determine the hydrogen peroxide solution Degradation products, for anthraquinone production of hydrogen peroxide enterprises in the working solution degradation and removal of reference.