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食品研究与开发:2017,38(19):139-142
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HPLC测定玉米中玉米赤霉烯酮和赭曲霉毒素A
郑睿行,周子焱,傅晓,林成栋,沈坚*
(宁波市食品检验检测研究院,浙江宁波315000)
Determination of Zearalenone and Ochratoxin A in Corn by Means of HPLC
ZHENG Rui-hang,ZHOU Zi-yan,FU Xiao,LIN Cheng-dong,SHEN Jian*
(Ningbo Institute for Food Control,Ningbo 315000,Zhejiang,China)
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投稿时间:2017-01-19    
中文摘要: 建立玉米中玉米赤霉烯酮(Zearalenone,ZEN)和赭曲霉毒素A(Ochratoxin A,OTA)的超高效液相色谱检测方法。样品用乙腈/水(90∶10,体积比)振荡提取,过滤后过真菌毒素净化柱,取上清液氮气吹干,用流动相溶解残渣,过0.22 μm有机滤膜于进样瓶,采用高效液相色谱检测法(High Performance Liquid Chromatography,HPLC)分析。在ZORBAX SB-C18反相柱上分离后,ZEN以甲醇/水(60∶40,体积比)作为流动相,OTA以乙腈/水/乙酸(43∶56∶1,体积比)为流动相,荧光检测器检测。ZEN的线性范围为0.5 μg/mL~6.0 μg/mL,相关系数大于0.99;OTA的线性范围为0.05 μg/mL~0.8 μg/mL,相关系数大于0.99。3个不同水平的加标平均回收率为86.4%~114.1%,相对标准偏差不大于10%。ZEN和OTA的检测限分别为5.0 μg/kg和1.0 μg/kg。应用该方法对收集的不同玉米样品进行测定,发现ZEN和OTA污染较严重,超标率均为71.4%。该方法具有操作简单、灵敏度高、重现性好等特点,能够用于玉米样品中真菌毒素的测定。
Abstract:Determination method of zearalenone(ZEN)and ochratoxin A(OTA)in corn by high-performance liquid chromatography (HPLC)was established.Acetonitrile/water(90 ∶10,volume ratio)for the extraction solvent extracted zearalenone and ochratoxin A in corn,clean-up column purification;then the supernatant was dried by nitrogen,with the mobile phase to dissolve the residue,through the 0.22 μm organic filter to the inlet,HPLC detection.Methanol/water(60∶40,volume ratio)was used as mobile phase for ZEN,and acetonitrile/water/acetic acid(43 ∶56 ∶1,volume ratio)for OTA.The linearity range of ZEN and OTA were 0.5 μg/mL-6.0 μg/mL and 0.05 μg/mL-0.8 μg/mL,respectively,with correlation coefficient>0.99.Recovery experiments were conducted by adding standard into the corn sample,with recoveries of 86.4%-114.1%,relative standard deviation of less than10%.The detection limit of ZEN and OTA were 5.0 μg/kg and 1.0 μg/kg,respectively.Different corn samples were found to be highly contaminated by ZEN and OTA using the method,with 71.4%of excessive rate.The method is simple and fast,good reproducibility,suitable for ZEN and OTA detection in the actual application.
文章编号:201719030     中图分类号:    文献标志码:A
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