高效液相色谱-串联质谱法同时测定地龙中4个黄曲霉毒素

目的: 建立同时测定地龙中4个黄曲霉毒素含量的高效液相色谱串联质谱法。 方法: 样品经甲醇-水(80∶20,v/v)提取,通过免疫亲和柱净化后,采用高效液相色谱串联质谱法测定其中4个黄曲霉毒素的含量,以多反应监测(MRM)方式分别监测离子对m/z 313→241(黄曲霉毒素B₁,CE 50 eV),m/z 315→259(黄曲霉毒素B₂,CE 43 eV),m/z 329→243(黄曲霉毒素G₁,CE 38 eV)和m/z 331→245(黄曲霉毒素G₂,CE 40 eV)。 结果: 黄曲霉毒素B₁、B₂、G₁、G₂的检测限分别为0.03,0.02,0.03,0.02 μg·kg^-1,回收率在88.0%~100.3%范围内,RSD均低于6.1%。 结论: 该方法快速、灵敏,结果准确,适用于地龙中4个黄曲霉毒素的同时检测。

Objective: To establish a sensitive and accurate liquid chromatography-tandem mass spectrometry method(LC-MS/MS) for simultaneous determination of four aflatoxins in Pheretima. Methods: The samples were firstly extracted with methanol-water solution(80∶20,v/v),and then cleaned up by immunoaffinity columns.The mass spectrometer was operated in the positive ionization electrospray(ESI) mode using multiple reaction monitoring(MRM) for analysis of four aflatoxins.The transitions of m/z 313→241 (aflatoxin B₁,CE 50 eV),m/z 315→259 (aflatoxin B₂,CE 43 eV),m/z 329→243 (aflatoxin G₁,CE 38 eV) and m/z 331→245(aflatoxin G₂,CE 40 eV) were used to quantify four aflatoxins,respectively. Results: The detection limits of aflatoxin B₁,B₂,G₁ and G₂ were 0.03,0.02,0.03 and 0.02 μg·kg^-1,respectively.The recoveries of four analytes ranged from 88.0% to 100.3% and the relative standard deviations were all below 6.1%. Conclusion: The method is sensitive,simple and accurate,and proved to be suitable for the simultaneous determination of four aflatoxins in Pheretima.