摘要
采用甲醇-水提取,C18小柱净化,反相HPLC荧光检测器测定了玉米、面粉、小麦样品中的玉米赤霉烯酮及其代谢物和黄曲霉B1。对样品预处理和高效液相色谱测定条件进行了优化,ZON,α-ZOL,β-ZOL和AFTB1的线性范围分别为5.0μg/L^146g/L,25.0μg/L^200g/L,25.0μg/L^160g/L和0.4μg/L^2.0g/L,检出限分别为0.5、2.5、2.5和0.04μg/kg;加标回收率在80.0%~110.0%范围内;日间相对标准偏差为4·5%~9.2%,日内精密度2.7%~7.4%。本方法灵敏准确,易于推广,适用于粮食中玉米赤霉烯酮及其代谢物的检测。
A reversed phase high performance liquid chromatographic (RP-HPLC) method for the determination of zearalenone and its metabolites in foodstuff was developed. The mycotoxins were extracted from foodstuff with aqueous 40% methanol and the extract was applied to a C18 cartridges, then eluted with methanol. The elutes were analyzed by RP-HPLC on a Phenomenx C18 eolunm(5μm, 250 mm×4.6 mm i. d. ) ; column temperature, 2.5℃ ; with, H2O/methanoL/acetonitrile(46: 10:44) as mobile phase( 1.0 mL/min) and fluorescence detection at 418 nm(λex= 236 nm). Calibration graphs were linear up to 146 mg/L for zearalenone (ZON) ,200 mg/L for α-zearalenol (α-ZOL) ,160 mg/L for β-zearalenol (β-ZOL) and 2 mg/L for Aflatoxin B1 ( AFT B1 ) The correlation coefficnts ranged from 0. 995 to 0. 999. The limits of detection for ZON, α-ZOL, β-ZOL, AFT B1 were 0.5 μg/kg, 2.5 μg/kg, 2.5μg/kg and 0.04 μg/kg, respectively. Recoveries of all compounds were in the range of 80.0% -110.0%. The intra-day precision was in the range of 4.5%-9.2%, the inter-day precision was in the range of 2.7% -7.4%. This sensitive and accurate method can be used for the determination of zearalenone and its metabolites in grains.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第3期351-354,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金重点(No.30030120)资助项目