摘要
为测定麦麸中黄曲霉毒素含量,试验建立了免疫亲和柱-高效液相色谱法。通过对10批样品检测结果的分析,初步考察了麦麸在黄曲霉毒素污染方面的安全性问题。样品经提取后,用免疫亲和柱净化,采用Syncronis C_(18)(250 mm×4.6 mm,5μm)色谱柱,以甲醇-乙腈-水(体积比30︰13︰57)为流动相,采用柱后碘衍生化法,用荧光检测器检测,激发波长为360 nm,发射波长为450 nm。黄曲霉毒素G_2、G_1、B_2、B_1分别在0.004~0.019μg·kg^(-1)(r=0.999 9),0.011~0.053μg·kg^(-1)(r=0.999 9),0.004~0.022μg·kg^(-1)(r=0.999 9)和0.010~0.051μg·kg^(-1)(r=0.999 9)范围内线性关系良好,AFB^4_1、AFB_2、AFG_1、AFG_2最低检出限分别为5.6×10^-,2.3×10^(-4),1.08×10^(-3)和4.3×10^(-4)μg·kg^(-1)。高中低不同浓度的黄曲霉毒素的加样回收率平均值分别为95.23,94.24和93.23μg·kg^(-1)。RSD(n=6)在0.54%~1.41%之间。10批样品中均检出黄曲霉毒素G_2,含量低于0.1μg·kg^(-1),有2批样品检出黄曲霉毒素G_2、B_2、B_1,黄曲霉毒素总量低于0.16μg·kg^(-1)。该方法经方法学验证,可用于麦麸中黄曲霉毒素检测。
A method had been developed for the aflatoxin in wheat bran by HPLC detection after immune affinity column purification.The safety of wheat bran in aflatoxin contamination was preliminarily investigated by analyzing the results of10 batches of samples.Samples after extraction,using immune affinity column purification and adopting Syncronis C18(250mm×4.6 mm,5μm)chromatographic column to detect,the mobile phase was methanol,acetonitrile and water(volume ratio of 30︰13︰57).The fluorescence detectorλex was set at 360 nm andλem was 450 nm.The linear ranges of aflatoxin G2,G1,B2and B1 were 0.004-0.019μg·kg-1(r=0.999 9),0.011-0.053μg·kg-1(r=0.999 9),0.004-0.022μg·kg-1(r=0.999 9)and 0.010-0.051μg·kg-1(r=0.999 9),respectively.The minimum detectable limits of AFB1,AFB2,AFG1 and AFG2 are 5.6×10-4,2.3×10-4,1.08×10-3,and 4.3×10-4μg·kg-1.In addition,the average value of the additive recovery of aflatoxin in different concentrations was 95.23,94.24 and 93.23μg·kg-1,respectively.RSD(n=6)was between 0.54%and 1.41%.Aflatoxin G2 was detected in 10batches of samples,the content was lower than 0.1μg·kg-1,2 batches of samples were detected with aflatoxin G2,B2 and B1,and the total amount of aflatoxin was lower than 0.16μg·kg-1.This method could be used for detection of aflatoxin in wheat bran.
作者
周欣
张琳
毛婵
张传辉
王云红
杨荣平
ZHOU Xin;ZHANG Lin;MAO Chan;ZHANG Chuanhui;WANG Yunhong;YANG Rongping(Southwest University,College of Pharmacy,Chongqing 400715;Chengdu University of Traditional Chinese Medicine,College of Pharmacy,Chengdu 610075;Chongqing Academy of Chinese Materia Medica,Chongqing 404100)
出处
《食品工业》
CAS
北大核心
2019年第2期327-330,共4页
The Food Industry
关键词
黄曲霉毒素
麦麸
免疫亲和柱-高效液相色谱法
aflatoxin
wheat bran
Immuno-affinity column and high performance liquid chromatography