UPLC-MS/MS法测定硫辛酸中催化剂四丁基溴化铵的残留量

UPLC-MS/MS determination of tetrabutyl ammonium bromide in lipoic acid

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 an UPLC-MS/MS method for determination of Tetrabutyl ammonium bromide（TBAB） in lipoic acid.Methods：A Waters Atlantis HILIC SILICA（2.1mm×100mm,3μm）column was used with acetonitrile-0.1mol·L-1 ammonium formate（pH=3.5）（95︰5）as the mobile phase.The flow rate was 0.2 mL·min-1.TBAB in lipoic acid extracted by chloroform-water（1︰1）was detected by UPLC-MS/MS.Result：The standard curve was linear over the range of 5-100ng·mL-1（r =0.996）,with the detection limit of 1×10-14g;The average recovery was 99.4%.Conclusion：this mothod is simple,rapid and precise enough to control the remain of TBAB in lipoic acid.