摘要
采用免疫亲和方法进行样品前处理,用甲醇一乙腈一水三元流动相体系分离黄曲霉毒素,氯化汞溶液在线衍生,荧光检测器检测,建立了新型的高效液相色谱柱后衍生测定黄曲霉毒素(B1、B2、G1、G2、M1)的方法。该方法在13min内完成测定,线性关系良好,5种黄曲霉毒素的线性相关系数r值均大于0.999。方法成功应用于花生、花生制品、大米、玉米等农产品。对样品进行不同水平的加标回收实验,回收率为83%-100%,相对标准偏差1.51%-4.98%(12=7),B,检出限(S/N=3)和定量下限(S/N=10)分别达到了0.05μg/kg和0.17μg/kg。
A new post-column derivatization method for the determination of aflatoxins( B1, Bz, G1, G2, and M1 ) by HPLC was developed. Sample was purified by immuno-affinity column and full separation of five aflatoxins could be achieved by the mobile phase composed of methanol - acetonitrile - water (22 : 18 : 60 by volume) within 13 min. Aflatoxins were enhanced by mercury chloride solvent on- line and detected by fluorescence detector. The calibration curve was linear in the range of 0. 5 - 60 μg/kg and the average correlation coefficients was of 0. 999 5. The new method was successfully applied to the analyses of aflatoxins in contaminated peanut, peanut products, rice, corn. Recoveries of aflatoxins spiked to peanut samples at different concentration levels were 83% - 100% with relative standard deviations of 1.51% -4.98% (n = 7 ). The limit of detection (S/N = 3 ) and the limit of quantification(S/N = 10) of aflatoxin B~ were 0. 05 μg/kg and 0. 17 μg/kg, respectively.
出处
《分析测试学报》
CAS
CSCD
北大核心
2007年第6期774-778,共5页
Journal of Instrumental Analysis
基金
国家科技部重点资助项目([2006]G003700)
湖北省及武汉市
中国农业科学院科技攻关项目(2006AA201B11
200720422135)