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免疫亲和柱净化-HPLC柱后光化学衍生荧光法测定花生饮料中的黄曲霉毒素B1

邹沫君1 ,陈 诚2

(1 乐山市食品药品检验检测中心,四川 乐山 614000;

2 山东高速四川产业运营公司,四川 乐山 614000)

摘 要:建立了免疫亲和柱净化-光化学衍生高效液相色谱荧光法测定花生饮料中黄曲霉毒素B1含量的方法。试 样经乙腈-水溶液(体积比 80∶20)提取,免疫亲和柱富集和净化后,采用 Thermo Syncronis C18色谱柱(250mm× 4.6mm,5μm),以甲醇-水(体积比55∶45)为流动相,等度洗脱,荧光检测器检测(Ex:360nm,Em:440nm)。结果表明: 黄曲霉毒素B1检出限为7.54×10-3 μg/kg;标准曲线的线性范围为0.1~20.0ng/mL(r=0.9999);3个不同水平的加标平均 回收率为96.88%~98.82%,RSD值为0.85%~1.07%。10批试样中黄曲霉毒素B1测定值为0~2.09μg/kg,均无过量 残留。该方法具有操作简便、灵敏度高、重现性佳等特点,适用于花生饮料中黄曲霉毒素B1的检测。

关键词:免疫亲和柱;高效液相色谱;光化学衍生;花生饮料;黄曲霉毒素B1

Determination of Aflatoxin B1 in Peanut Beverage by HPLC-FLD with Photochemical Derivatization after Immunoaffinity Column Purification

ZOU Mo-jun1 ,CHEN Cheng2

(1 Leshan Center for Food and Drug Control,Leshan 614000,China;

2 Shandong Highspeed Sichuan Industrial Operation Company,Leshan 614000,China)

Abstract: A method was developed for determination of aflatoxin B1 in peanut beverage by HPLC- FLD with photochemical derivatization after immunoaffinity column purification. In the experiments, the samples were extracted by acetonitrile-water(80∶20v/v),then the extract was purified by immunoaffinity column,and aflatoxin B1 was separated by reversed-phase HPLC,and then quantified with fluorescence detection(Ex:360nm,Em:440nm), and the separation was performed on a Thermo Syncronis C18 Column(250mm×4.6mm,5μm)with isocratic elution of methanol-water(55∶45v/v). The detection limits were 7.54×10-3 μg/kg for AFT B1. The calibration curve of AFT B1 was achieved in the concentration range of 0.1~20.0ng/mL(r=0.9999). The recovery of AFT B1 spiked to peanut beverage was within 96.88%~98.82% and the relative standard deviations were between 0.85% to 1.07%. 10 samples measured value is 0~2.09μg/kg for AFT B1,and all samples have no excessive additives. The method is simple and convenient,good reproducibility,suitable for AFT B1 determination in peanut beverage.

Key words: immunoaffinity column;high performance liquid chromatography;photochemical derivatization;peanut beverage;aflatoxin B1

中图分类号:TS207.3 文献标志码:A 文章编号:1007-7871(2020)04-0030-05

(2020年 第23卷 第4期)

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