摘要
研究建立同时检测啤酒及酿造原料中黄曲霉毒素 B1、玉米赤霉烯酮和赭曲霉毒素 A 的免疫亲和柱净化-柱后化学衍生-高效液相色谱方法。样品经过甲醇-水（80:20,v/v）提取，通过免疫亲和柱富集和净化，采用 Thermo BDS HYPERSIL C18 色谱柱，以乙腈-2%乙酸（40:60,v/v）为流动相，等度洗脱，柱后以 0.5%碘溶液衍生、改变波长荧光检测。黄曲霉毒素 B1、玉米赤霉烯酮和赭曲霉毒素 A 检出限分别为 0.05μg/ kg（AFB1）、3.19μg/ kg（ZEA）和 0.22μg/ kg (OTA)，标准曲线的线性范围分别为 0.2～10.0、10.0～1000.0 和 5.0～50.0 μg/L；在大麦样品中加标回收率为 90.0%～109.5%，相对标准偏差为 2.18%～4.94%。被检 37 个样品的真菌毒素含量检测结果表明正常贮存下的啤酒原料均未检测出真菌毒素，但在霉变大麦样品中可以检测出少量的真菌毒素。
A method was developed for simulataneous determination of aflatoxins B1, zearalenone and ochratoxin A in brewing grains by HPLC after immunoaffinity column clean-up and post-column derivatization. In the experiments, the samples were extracted by methanol-water(80∶20,v/v), then the extract was purified by immunoaffinity column, and the three toxins were separated by reversed-phase HPLC, and then quantified with fluorescence detection after chemical derivatization with 0.5 % iodine solution, and the separation was performed on a BDS HYPERSIL C18Column with isocratic elution of acetonitrile-2 % acetic acid(40∶60,v/v). The detection limits were 0.05 μg/ kg for AFB1, 3.19 μg/ kg for ZEA and 0.22 μg/ kg for OTA.The calibration curves of the three toxins were achieved in the concentration range of 0.2 ~10.0 for AFB1, 10.0 ~1000.0 for ZEA and 5.0~50.0 μg/L for OTA. The recoveries of AFB1, ZEA and OTA spiked to barley was within 90.0 %~109.5 % and the relative standard deviations were between 2.18 % to 4.94 %. 37 samples collected including barley, malt, wheat, corn starch and hops were measured by such method, and the results showed that no mycotoxins detected in all the brewing materials in good storage conditions, but could be detected in low level in mildewed barley.
出处
《酿酒科技》
北大核心
2014年第2期83-86,89,共7页
Liquor-Making Science & Technology
关键词
免疫亲和柱
柱后衍生
高效液相色谱
真菌毒素
啤酒酿造原辅料
immunoaffinity column
chemical derivatization
high performance liquid chromatography
mycotoxin
brewing grains
beer
