快速液相色谱-串联质谱法测定果实类药材中的黄曲霉毒素

Determination of Aflatoxins in Fruit Traditional Chinese Medicines by Rapid-Resolution Liquid Chromatography Tandem Mass Spectrometry

目的建立中药材中4种黄曲霉毒素测定的快速液相色谱-串联质谱方法。方法样品经体积分数70%甲醇提取、免疫亲和柱净化,岛津Shim-pack XR-ODS色谱柱,用甲醇-乙腈(1∶1)和水为流动相,梯度洗脱,ESI+扫描,多反应监测(MRM)。结果黄曲霉毒素B1在0.102 1～10.21 ng.mL-1内、黄曲霉毒素B2在0.061 2～7.65 ng.mL-1内、黄曲霉毒素G1在0.193～9.65 ng.mL-1内、黄曲霉毒素G2在0.121～7.55 ng.mL-1内,线性关系均良好,r>0.999 8;4种黄曲霉毒素回收率在77.0%～102.4%之间。结论本方法准确可靠,适合中药材中4种黄曲霉毒素含量的测定。

OBJECTIVE To develope a method for determination of four aflatoxins （ B1 , B2, G1 , G2 ） in fruit traditional Chinese medicines by rapid-resolution liquid chromatography coupled with electrospray ionization triple quadrupole tandem mass spectrometry. METHODS After being extracted with 70% methanol and purified by immunoaffinity columns, the four aflatoxins were separated on a Shim-pack XR-ODS column using gradient elution with the mobile phase of CH3 CN-CH30H-H20 mixtures monitored under MRM mode in ESI positive scan. RESULTS There was a good linear relationship over the range of 0. 102 1 - 10. 21 ng·mL^-1 for AFB1 , 0. 061 2 -7.65 ng·mL^-1 for AFB2, 0. 193 -9. 65 ng·mL^-1 for AFG1, 0. 121 -7.55 ng·mL^-1 for AFG2 （r 〉 0. 999 8） , respec- tively. The average recoveries ranged from 77. 0% - 102. 4%. CONCLUSION This method provides a simple and feasible way to determine aflatoxins.