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目的:建立超高效液相色谱-质谱联用(UPLC-MS/MS)检测硫辛酸原料药中催化剂四丁基溴化铵残留量的方法。方法:色谱柱为W aters Atlantis H ILIC S ilica(2.1mm×100mm,3μm),流动相:乙腈-0.1mol.L-1甲酸铵溶液(pH=3.5)95:5,流速0.2mL.min-1。经氯仿和水(1:1)提取出的四丁基溴化铵通过UPLC-MS/MS进行检测。结果:本法的线性范围为5～100ng.mL-1(r=0.996);最低检测限为1×10-14g;回收率为99.4%。结论:本法操作简便,结果准确,可用于硫辛酸中催化剂四丁基溴化铵的质量控制。
OBJECTIVE: To establish a method for the determination of the catalyst tetrabutyl ammonium bromide in lipoic acid raw material by ultra performance liquid chromatography-mass spectrometry (UPLC-MS / MS). METHODS: The column was Watsters Atlantis HILIC Sialica (2.1 mm × 100 mm, 3 μm). The mobile phase was acetonitrile-0.1 mol·L-1 ammonium formate solution (pH = 3.5) 1. Tetrabutylammonium bromide extracted by chloroform and water (1: 1) was detected by UPLC-MS / MS. Results: The linear range of this method was 5 ~ 100 ng.mL-1 (r = 0.996). The detection limit was 1 × 10-14 g. The recovery was 99.4%. Conclusion: The method is simple, accurate and can be used for the quality control of tetrabutylammonium bromide in lipoic acid.