摘要
建立一种液液萃取净化,结合柱后碘衍生-高效液相色谱检测食品中黄曲霉毒素B1的新方法。食品中黄曲霉毒素B1采用乙腈-水(85︰15, V/V)混合溶液提取,加入蛋白沉淀剂和正己烷除去蛋白质及脂溶性杂质,经三氯甲烷萃取净化、浓缩及定容后用柱后碘衍生-高效液相色谱荧光检测器进行检测。结果表明,在0.1~50.0 ng/mL浓度范围内,线性关系良好,拟合系数为0.999 97,在3倍信噪比下计算方法检出限为0.02μg/kg;分别对多种样品进行低(0.4μg/kg)、中(4.0μg/kg)、高(40μg/kg)加标回收率试验,回收率范围为75.9%~94.7%,相对标准偏差(RSD, n=6)为0.1%~5.4%。该方法分析速度快,准确度高,重复性好,适用于食品中黄曲霉毒素B1的检测。
To establish a new method for the determination of aflatoxin B1 in food by post column iodine derivatizationhigh performance liquid chromatography with liquid-liquid extraction purification, aflatoxin B1 in food was extracted by acetonitrile-water(85︰15, V/V) mixed solution, then protein precipitator and n-hexane were added to remove proteins and lipid soluble impurities. The extracts were further purified by trichloromethane with liquid-liquid extraction, and which was concentrated and volume fixed. Aflatoxin B1 was determined by post column iodine derivatization-high performance liquid chromatography with fluorescence detector. The results showed that within the concentration range of 0.1-50.0 ng/mL, the linear relationship was good and the fitting coefficient was 0.999 97. The detection limit of this method was 0.02 μg/kg with signal to noise(S/N) ratio of 3. The standard recovery rates of various samples were tested, the recovery rates of different level(0.4, 4.0 and 40 μg/kg) were 75.9%-94.7% and the relative standard deviation(RSD, n=6) was 0.1%-5.4%. The proposed method was rapid, accurate and repeatable, which was suitable for the detection of aflatoxin B1 in food.
作者
马海峰
陶唐平
方林明
刘成林
单平平
陈辉德
MA Haifeng;TAO Tangping;FANG Linming;LIU Chenglin;SHAN Pingping;CHEN Huide(Anhui Zhongchuang Food Testing Co.,Ltd.,Wuhu 241000)
出处
《食品工业》
CAS
北大核心
2020年第5期296-299,共4页
The Food Industry
关键词
食品
黄曲霉毒素B1
液液萃取净化
柱后碘衍生
高效液相色谱荧光检测器
food
aflatoxin B1
liquid-liquid extraction purification
post column iodine derivatization
high performance liquid chromatography with fluorescence detector
