食品科学 ›› 2011, Vol. 32 ›› Issue (12): 254-258.doi: 10.7506/spkx1002-6630-201112056

• 分析检测 • 上一篇    下一篇

高效液相色谱和高效液相色谱-离子阱质谱测定花生、玉米和大米中黄曲霉毒素方法比较

范素芳,李培武,*,王秀嫔,丁小霞,张 文,张 奇   

  1. 1. 中国农业科学院油料作物研究所
    2.农业部油料作物生物学重点开放实验室 3.农业部油料及制品质量监督检验测试中心
  • 出版日期:2011-06-25 发布日期:2011-06-10
  • 基金资助:
    农业部“948”项目(2010-G1);中国农业科学院所长基金项目(SZ-2010-3);国家自然科学基金项目(31000787); 国家现代农业(油菜)产业体系建设专项(nycytx-005);“十一五”国家科技支撑计划项目(2010BAD01B07); “十二五”国家科技支撑计划项目(2011BAD02D02)

Comparison on Determination of Aflatoxins in Peanut, Corn and Rice by Liquid Chromatography and Liquid Chromatography-Tandem Mass Spectrometry

FAN Su-fang1,LI Pei-wu1,2,3,*,WANG Xiu-pin1,2,DING Xiao-xia1,3,ZHANG Wen1,3,ZHANG Qi1,3   

  1. 1. Institute of Oil Crops Research, Chinese Academy of Agricultural Sciences, Wuhan 430062, China;2. Key Laboratory of Oil Crop Biology, Ministry of Agriculture, Wuhan 430062, China;3. Quality Inspection and Test Center for Oilseeds Products, Ministry of Agriculture, Wuhan 430062, China
  • Online:2011-06-25 Published:2011-06-10

摘要: 比较花生、玉米和大米中黄曲霉毒素(AFT)测定的两种分析方法。样品经70%甲醇溶液(含NaCl 4g/100mL)提取,自制免疫亲和柱净化。洗脱液一分为二,一份经正己烷、三氟乙酸衍生后用配有荧光检测器的液相色谱检测;另一份无需衍生用液相色谱-串联离子阱质谱检测。液相色谱测定的AFB1、AFB2、AFG1和AFG2的检出限(RSN=3)分别为0.5~1.5μg/kg,相关系数在0.9979~0.9999,加标回收率50.29%~126.54%;液相色谱-串联质谱测定的AFB1、AFB2、AFG1和AFG2的检出限分别为0.1~0.2μg/kg;相关系数在0.9993~0.9998,加标回收率50.38%~121.27%。结果表明液相色谱-离子阱质谱法无论在选择性还是在灵敏度上都优于高效液相色谱。

关键词: 液相色谱, 黄曲霉毒素, 液相色谱-电喷雾线性离子阱质谱, 方法比较

Abstract: Two different analytical methods for determining aflatoxins in peanut, corn and rice were compared in this paper. Samples were extracted by 70% methanol supplemented with 4 g/mL NaCl and cleaned up by immunoaffinity columns. Half part of the eluent was derivated with hexane and trifluoroacetic acid, and detected by liquid chromatography with fluorescence detection (FLD), the rest part of the eluent was detected by liquid chromatography-electrospray ionization tandem linear ion trap mass spectrometer (LC-ESI-LTQ). Limits of detection (LOD) of AFB1, AFB2, AFG1 and AFG2 determined by LC-FLD were in the range of 0.5-1.5μg/kg, the correlation coefficients were in the range of 0.9979-0.9999, and the recovery rates of spiked samples were in the range of 50.29%-126.54%; LODs of AFB1, AFB2, AFG1 and AFG2 determined by LC-ESI-LTQ were in the range of 0.1-0.2μg/kg, the correlation coefficients were in the range of 0.9993-0.9998, and the recovery rates of spiked samples were in the range of 50.38%-121.27%. All results showed that liquid chromatography-electrospray ionization tandem linear ion trap mass spectrometric method was more selective and sensitive for the analysis and confirmation of aflatoxins in peanut, corn and rice than LC-FLD.

Key words: aflatoxin, liquid chromatography, liquid chromatography-electrospray ionization tandem linear ion trap mass spectrometer (LC-ESI-LTQ), method comparison

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