免疫亲和柱净化-在线柱后光化学衍生-HPLC-FLD同时测定甘草中黄曲霉毒素B_1,B_2,G_1,G_2和赭曲霉毒素A的含量

Simultaneous determination of aflatoxin B_1,B_2,G_1,G_2 and ochratoxin A in Glycyrrhiza uralensis by HPLC-FLD after immunoaffinity column with online post-column photochemical derivatization

目的:建立同时检测甘草中黄曲霉毒素B1,B2,G1,G2和赭曲霉毒素A的免疫亲和柱净化-在线柱后光化学衍生-HPLC-FLD测定的方法。方法:样品经甲醇-水(80∶20)超声提取后,用免疫亲和柱净化和富集;以甲醇和0.5%乙酸溶液为流动相进行梯度洗脱,通过柱后光化学衍生,荧光检测器测定。结果:黄曲霉毒素G2,G1,B2,B1和赭曲霉毒素A的检测限分别为0.02,0.06,0.015,0.03,0.25μg.kg-1,平均加样回收率为76.0%～103%,RSD低于13%。结论:该方法快速简便、准确,可用于甘草中同时测定黄曲霉毒素B1,B2,G1,G2和赭曲霉毒素A的含量。

Objective： To develop a method for tile simultaneous determination of aflatoxin B1 , B2 , G1, G2 and ochratoxin A in Glycyrrhiza uralensis by HPLC-FLD after immunoaffinity column with online post-column photochemical defivatization. Method： Sample was extracted with MeOH： H20 （80： 20） and cleaned up by immunoaffinity column. The toxins were separated by reversedphase HPLC and the mobile phase was consisted of methanol and 0. 5% acetic acid solution with gradient elution. The determination was carried out by fluorescence detector after photochemical derivatization. Result： The detection limits of aflatoxin G2, G1, B2, B1 and ochratoxin A were 0.02, 0. 06, 0. 0!5, 0. 03 and 0. 25 μg·kg^-1 , respectively. The recoveries of analytes were from 76. 0% to 103% and the relative standard deviations （RSDs） were below 13%. Conclusion： The method is a simple, accurate and can be used to determine the contents of aflatoxin B1, B2, G1 , G2 and ochratoxin A in G. uralensis simultaneously.