高效液相色谱-柱后光化学衍生法测定参苓白术散中黄曲霉毒素G_2、G_1、B_2、B_1  

Determination of Aflatoxin G_2,G_1,B_2,B_1 in Shenling Baizhu Powder by HPLC with Post Column Photochemical Derivatization

作　　者：刘宁[1] 王萌萌[2] 金红宇[3] 孙磊[3] 刘德海[1] 乔菲[3] 

机构地区：[1]北京普析通用仪器有限责任公司,北京101200 [2]北京市药品检验所 [3]中国食品药品检定研究院

出　　处：《中国药事》2012年第5期442-445,共4页Chinese Pharmaceutical Affairs

基　　金：国家"十一五"科技支撑项目(编号2008BAI55B02);国家"重大创新药创制"科技重大专项(编号2009ZX09308-006)

摘　　要：目的建立中成药参苓白术散中黄曲霉毒素G2、G1、B2、B1的测定方法。方法样品经70%甲醇提取,免疫亲和柱净化后,采用高效液相色谱-柱后光化学衍生-荧光检测法定量,以串联质谱法验证。结果高效液相色谱法线性关系良好(r>0.999),回收率范围76.8%～115.2%(RSD范围1.8%～12.9%),检测了57批样品,并使用串联质谱仪的多反应监测模式确证了阳性结果。结论本法快速、简便、灵敏、准确,专属性强,可用于参苓白术散中黄曲霉毒素的检测。Objective To establish a method for determination of aflatoxin G2, G1, B2, B1 in Shenling Baizhu Powder. Methods The samples were extracted with 70% methanol and purified with immunoaffinaty column. Aflatoxins were determined by high-performance liquid chromatography- fluorescence detector with post column photochemical derivatization, and identified by liquid chromatography-tandem mass spectrometry. Results The quantitative analysis showed a good linear relationship （r〉0. 999）. The recoveries were between 76.8~ ~ 115.2% （RSD 1.8% - 12.9%）. Fifty- seven batches of sample were analyzed with the established method and the positive results were confirmed by tandem mass spectrometry in multiple reaction monitor mode. Conclusion The method is rapid, simple, accurate, sensitive specific for determination of aflatoxins in Shenling Baizhu Powder.

关 键 词：中成药 参苓白术散 黄曲霉毒素 免疫亲和柱 高效液相色谱 柱后光化学衍生 串联质谱 

分 类 号：R927.11[医药卫生—药学] R917