食品科学 ›› 2007, Vol. 28 ›› Issue (4): 241-245.

• 分析检测 • 上一篇    下一篇

毛细管气相色谱法测定小麦和玉米中脱氧雪腐镰刀菌烯醇

 黄志兵, 游淑珠, 邓舜洲, 许杨   

  1. 南昌大学中德联合研究院 南昌大学食品科学教育部重点实验室; 南昌大学中德联合研究院; 南昌大学食品科学教育部重点实验室; 江西 南昌 330047;
  • 出版日期:2007-04-15 发布日期:2011-12-31

Determination of Deoxynivalenol in Wheat and Corns by Capillary Gas Chromatography

 HUANG  Zhi-Bing, YOU  Shu-Zhu, DENG  Shun-Zhou, XU  Yang   

  1. Key Laboratory of Food Science,Ministry of Education,Sino-Germany Joint Research Institute,Nanchang University,Nanchang 330047,China
  • Online:2007-04-15 Published:2011-12-31

摘要: 本文采用毛细管气相色谱法测定了小麦和玉米中脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)的含量,小麦、玉米样品分别用乙腈-水(84:16,V/V)提取,小麦样品提取液用硅镁型吸附剂净化,玉米样品提取液用硅镁型吸附剂和活性炭二步净化,采用N-七氟丁酰咪唑(HFBI)为衍生剂,带电子捕获检测器的GC进行检测。DON加标量为0.5~1.5mg/kg时,5次重复实验的平均回收率:小麦样品为82.2%~98.5%,玉米样品为86.0%~103.4%,相对标准偏差(RSD)分别为6.2%~7.6%和6.4%~8.0%,该法DON的最低检出限为0.01mg/kg,线性范围为0.075~15mg/k8。用该法对21个小麦样品与20个玉米样品中DON的含量进行检测,其中小麦样品中DON含量为0.153~4.618mg/kg,污染率为47.6%,超标率为9.5%;而玉米样品中DON含量为0.116~3.004mg/kg,污染率为85%,超标率为20%。

关键词: 毛细管气相色谱法, 衍生, 脱氧雪腐镰刀菌烯醇, N-七氟丁酰咪唑, 谷类作物

Abstract: A determination method of deoxynivalenol(DON)in wheats and corns by capillary gas chromatography was studied. Samples were extracted with acetronile-water(84:16,V/V).The wheats liquid extracts were then purified by Florisil columns, while the corn liquid extracts were purified by a two-step procedure with both Florisil and active carbon columns.The final extract was then derivatized with N-heptafluorobutyrylimidazole(HFBI)and quantitated by GC with electron capture detector(GC- ECD).Recoveries of DON were spiked at 0.5~1.5 mg/kg ranged from 82.2% to 98.5% for wheat and from 86.0% to 103.4% for corn,with relative standard deviations of 6.2%~7.6% and 6.4%~8.0%,respectively.The limit of detection(S/N=3:1) of this method is 0.01 mg/kg for DON.The linearity of the detector response is proper in 0.075~15 mg/kg.21 wheat and 20 corn samples were analysed by GC-ECD,whereas 10 wheat samples are found contaminated with DON in 0.153~4.618 mg/kg.17 corn samples are found contaminated with DON in 0.116~3.004 mg/kg.

Key words: capillary gas chromatography, derivatized, deoxynivalenol, N-heptafluorobutylimmidazole, cereals