高效液相色谱/离子阱质谱快速鉴定茚满二酮类鼠药

目的建立鼠药药饵中4种茚满二酮类鼠药的高效液相色谱/离子阱质谱快速鉴定方法。方法鼠药药饵经丙酮提取后,采用固相萃取净化,选择液相色谱/离子阱质谱仪(LC-IT/MS)的最佳仪器条件,进行液相色谱的分离和二级质谱的裂解,根据质谱分析三离子原则进行定性。结果 4种茚满二酮类鼠药的二级质谱碎片离子具有较好的特征性和稳定性,母离子和子碎片离子的关系清晰,敌鼠的定性离子对为m/z339→167和m/z339→145,氯敌鼠为m/z373→201和m/z373→145,异杀鼠酮为m/z229→145和m/z229→187,杀鼠酮为m/z229→172和m/z229→145。结论本实验建立的方法简便,结果准确可靠,适合于茚满二酮类鼠药的定性鉴别。

Rapid qualitative analysis of indandione rodenticides by high-performance liquid chromatography coupled with ion trap mass spectrometry

Objective To establish a method for the simultaneous qualitative analysis of four indandione rodenticides by high-performance liquid chromatography coupled with ion trap mass spectrometry(LC-IT/MS).Methods After the indandione rodenticides in bait were extracted by acetone,and cleaned by solid-phase extraction(SPE),the liquid chromatographic separation and the MS/MS cracking were performed in the optimal instrument conditions by LC-IT/MS.Qualitative detection were carried out by the principle of mass spectrometry analysis of three qualitative ions.Results The MS/MS fragment ions had good characteristics and stability,the cracking ways to the parent ions and fragment ions were clear.Qualitative ion pairs were m/z 339→167 and m/z 339→145 for diphacine,m/z 373→201 and m/z 373→145 for chlorophacinone,m/z 229→145 and m/z229→187 for valone,and m/z 229→172 and m/z229→145 for pindone.Conclusion This established method is simple,accurate and reliable for the qualitative analysis of indandione rodenticides.