Determination of cardiotoxin in serum by ultra-high performance liquid chromatography tandem with mass spectrometry
Objective To develop a new method for the determination of cardiotoxin in serum by ultra-high performance liquid chromatography tandem with mass spectrometry(UPLC-MS-MS).Methods Totally 100 μl serum sample was precipitated with 300 μl acetonitrile for 2 h at-20 ℃ and then separated by high speed centrifugation for 10 min.The upper organic phase was diluted at 1:1 by pure water,then passed through the membrane,and measured it by UPLC-MS-MS.Separation of the sample was achieved by a Protein BEH C4 column with a gradient elution of 0.1％formic acid aqueous solution-0.1％formic acid acetonitrile solution.The column temperature was 70 ℃.The concentration of cardiotoxin was measured by electrospray ion source(ESI)with positive ion mode and quantified by external standard method.Results This method showed a good linearity for cardiotoxin in the range of 2.0-200.0 μg/L,r=0.999 2.The recovery was in the range of 98.6％-115.0％with RSDs of 3.6％-9.8％.The limit of detection was 0.6 μg/L.Conclusion This method is simple to operate and has high sensitivity and accuracy,and is applicable to rapid detection of cardiotoxin in the serum.
万方数据
维普
