免疫亲和柱净化-柱前衍生-高效液相色谱法测定中药薏苡仁中的伏马毒素  

Determination of Fumonisins in Coix Seed by HPLC Coupled with Immunoaffinity Column Purification-Precolumn Derivatization

作　　者：张太 毛丹 王少敏 刘贤贤 周恒 季申 ZHANG Tai;MAO Dan;WANG Shaomin;LIU Xianxian;ZHOU Heng;JI Shen(School of Pharmacy,Shanghai University of Traditional Chinese Medicine,Shanghai 201203;Shanghai Institute for Food and Drug Control,NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai 201203)

机构地区：[1]上海中医药大学中药学院,上海201203 [2]上海市食品药品检验研究院国家药品监督管理局中药质量控制重点实验室,上海201203

出　　处：《分析科学学报》2022年第2期233-236,共4页Journal of Analytical Science

基　　金：国家科技部重点研发计划(No.2017YFC1700800);国家自然科学基金(No.81803719);上海市科委研发平台专项(No.18DZ2292200);上海市科委技术标准专项(No.18DZ2200900)。

摘　　要：建立了免疫亲和柱净化-自动化柱前衍生-高效液相色谱测定中药薏苡仁中伏马毒素(FB_(1)、FB_(2)、FB_(3))的分析方法。样品经甲醇-乙腈-水(1∶1∶2)振荡提取,免疫亲和柱净化,采用自动化柱前衍生-高效液相色谱测定FB_(1)、FB_(2)、FB_(3)。结果表明:FB_(1)、FB_(2)、FB_(3)在5~200 ng/mL之间线性关系良好,相关系数均大于0.999;对阴性样品分别添加50、250、1 000μg/kg低中高3个水平进行加标回收实验,回收率分别为75.1%~81.6%、85.4%~91.7%和78.6%~84.3%,相对标准偏差(RSD)均小于4%;检测限分别为6、10、10μg/kg;定量限分别为20、30、30μg/kg。此方法简便快速、灵敏度高、重复性好,可用于中药薏苡仁中伏马毒素的准确定量。A method for the determination of fumonisins B_(1),B_(2) and B_(3) in Coix seed by high performance liquid chromatography(HPLC) was established.The sample was extracted by methanol acetonitrile water(1∶1∶2) and purified by immunoaffinity column,and the fumonisins B1,B2 and B3 were determined by automatic precolumn derivatization method.The developed method had a good linear relationship for fumonisins B1,B2 and B3 in the concentration range of 5-200 ng/mL,and the correlation coefficients were all over 0.999.The recoveries of fumonisins B_(1),B_(2) and B_(3) were 75.1%-81.6%,85.4%-91.7% and 78.6%-84.3% with RSD less than 8%.The limits of detection were 6 μg/kg and 10 μg/kg,respectively.The limits of quantitation were 20 μg/kg,30 μg/kg and 30 μg/kg,respectively.The method is simple,rapid,sensitive and reproducible,and can be used for the accurate quantification of fumonisins in coix seed.

关 键 词：伏马毒素 薏苡仁 液相色谱 自动进样程序 

分 类 号：O657.72[理学—分析化学]