摘要
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.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2012年第1期65-68,共4页
Chinese Pharmaceutical Journal
基金
国家科技重大专项-重大新药创新课题(中药中有害残留检测技术标准平台课题编号2009ZX09308-006)资助项目