固相萃取-超高效液相色谱串联质谱法测定牛奶中6种头孢菌素类抗生素

Determination of 6 kinds of cephalosporins in milk by solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry

目的建立固相萃取超高效液相色谱串联质谱(SPE-UPLC-MS/MS)同时检测牛奶中6种头孢菌素类抗生素含量的方法。方法样品经0.05 mol/L的磷酸氢二钾缓冲溶液提取,HLB固相萃取柱净化,液相色谱串联质谱法测定,采用多反应监测模式进行定性和定量分析。结果 6种头孢菌素类抗生素的检出限(S/N=3)和定量限(S/N=10)范围分别为0.05~0.4μg/kg和0.1~1.6μg/kg。样品加标回收率范围为66.3%~110.0%。结论该方法便捷、快速、高效,能够满足牛奶中头孢菌素类抗生素的检测。

Objective To developed a method for the detection of 6 kinds of cephalosporins in milk by solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS). Methods The samples were extracted with 0.05 mol/L phosphate buffer solution, cleaned up by HLB solid phase extraction column, and then analyzed by UPLC-MS/MS with multiple reaction monitoring(MRM) mode. Results The LODs and LOQs of 6 kinds of cephalosporins were in the ranged of 0.05~0.4 μg/kg and 0.1~1.6 μg/kg, respectively, with the mean recoveries varied from 66.25% to 109.97%. Conclusion The established method is simple, rapid and effective, and suitable for the determination of 6 kinds of cephalosporins in milk samples.