摘要
考察3种前处理方法的净化效果,建立柱后光化学衍生-高效液相色谱法对粮食中黄曲霉毒素B1的检测方法。样品经甲醇+水(70∶30)提取,常规手动亲和柱净化、全自动亲和柱净化及免疫磁珠-全自动净化3种前处理净化,经Eclipse plus C_(18)色谱柱分离,用64%水+18%甲醇+18%乙腈等度洗脱。优化色谱条件后,从加标回收率、实样检测、检测时长、操作步骤及净化效果等多个角度考察了这3种前处理方法对粮油中黄曲霉毒素B_(1)的残留净化效果的影响。结果表明:黄曲霉毒素B_(1)含量在0.677~21.660 ng/mL的范围内线性关系良好,其相关系数为0.99997,检出限为0.029μg/kg,定量限为0.097μg/kg;在5.0、10.0、20.0μg/kg加标水平下,黄曲霉毒素B_(1)加标回收率为82.1%~99.2%,3次重复测定的相对标准偏差不超过8.8%,3种前处理方法均满足粮油中黄曲霉毒素B_(1)的检测要求;3种前处理方法比较研究发现常规手动亲和柱净化和免疫磁珠-全自动净化的效果更加突出,其中免疫磁珠-全自动净化可实现重复利用,且快速简便、定量准确。
The purification effects of three sample pretreatments were investigated,and a method for the determination of aflatoxin B1 in cereals and oils by post-column photochemical derivatization high performance liquid chromatography was established.The samples were extracted with methanol and water(70∶30),purified by standard manual immunoaffinity column,automated immunoaffinity column and automated immunomagnetic beads,the separation of aflatoxins was performed on an Eclipse plus C_(18) column using isocratic elution with 64%water+18%methanol+18%acetonitrile.After the chromatogram spectrometry was optimized,the effects of these three sample pretreatments on the purification effect of aflatoxins in cereals and oils were investigated from multiple aspects:recovery,sample detection,length of detection,operation steps and purification efficiency.The results indicated that aflatoxin B_(1) had a good linear relationship in the range of 0.677~21.660 ng/mL,with the correlation coefficient of 0.99997,and the limits of detection and limits of quantitation were 0.029μg/kg and 0.097μg/kg.The recovery rate ranged from 82.1%to 99.2%for three different concentration levels,and RSDs were not larger than 8.8%.The three sample pretreatments for determining aflatoxin B_(1) could meet the need of cereals and oils inspection.Three methods of pretreatment were compared and the results of standard manual immunoaffinity column purification and automated immunomagnetic beads purification had better purification effect.Among them,automated immunomagnetic beads purification had the advantages of reutilization,simplicity,rapidity,and could accurately and quantitatively determine aflatoxin B_(1) in cereals and oils.
作者
黄力
杨静
李滑滑
洪玲
沈娜
曾奎杰
Huang Li;Yang Jing;Li Huahua;Hong Ling;Shen Na;Zeng Kuijie(Hunan Provincial Center for Monitoring of Grain Oil Products Quality,National Engineering Laboratory for Deep Processing of Rice and Byproducts,Changsha 410201)
出处
《中国粮油学报》
CAS
CSCD
北大核心
2022年第1期182-186,共5页
Journal of the Chinese Cereals and Oils Association
关键词
黄曲霉毒素B_(1)
免疫磁珠
亲和柱
自动化净化
高效液相色谱
aflatoxin B_(1)
immunomagnetic beads
immunoaffinity column
automatic purification
high performance liquid chromatography
