小麦中赭曲霉毒素A含量测定方法的改进研究  

Improvement the Determination Method of Wheat's Ochratoxin A

作　　者：和霁恬 邵志凌 放茂良 He Jitian;Shao Zhiling;Fang Maoliang(Food and Oil Science Research Institute of Yunnan Province/Yunnan Grain and Oil Products Quality Supervision and Testing Center,Kunming ,Yunnan 53003)

机构地区：[1]云南省粮油科学研究院/云南省粮油产品质量监督检验测试中心,云南昆明650033

出　　处：《粮食科技与经济》2018年第1期71-73,共3页Food Science And Technology And Economy

摘　　要：目的:优化GB 5009.96-2016中赭曲霉毒素A检测的前处理方法和色谱条件,以适应大批量样本的检测。方法:样品经甲醇:水(V∶V=80∶20)漩涡提取、免疫亲和层析净化,超高效液相色谱法测定。色谱条件为Thermo Scientific Hypersil GOLD C18反相柱(100mm×2.1mm,粒径1.9μm),流动相为1%乙酸水-乙腈(V∶V=60∶40),流速为0.25m L/min,进样量4μL,柱温:25℃,荧光检测激发波长333nm,发射波长460nm。结果:赭曲霉毒素A在1.00~20.00ng/m L时具有良好的线性关系,相关系数R2=0.999 7,加标回收率为82.9%~90.1%,精密度RSD5.1%~6.1%。本方法实验用时和流动相用量分别比国标法减少72.8%和87.5%。结论:本方法适用于小麦中赭曲霉毒素A含量的测定且更灵敏、高效和环保。在大批量样品分析中可有效节约时间、材料成本。Purpose： the pre-treatment and chromatographic condition of Ohratoxin A in GB 5009.96-2016 was improved to the bulk sample detection.Method： the samples were extracted by methanol/water （80∶20,V∶V）,extract by swirl extraction,cleared up with the immuno-affinity column.The contents of Ohratoxin A were determinated with improved ultra performance liquid chromatography.The separation of targeted compound was performed on Thermo Scientific Hypersil GOLD C18 （100 mm×2.1 mm,1.9 μm）, using water ：acetic acid ： acetonitrile （59.4∶0.6∶40,V∶V∶V）, as mobile phase with a flow rate of 0.25 mL/min at 25 ℃. The injection volume was 4 μL and detection conditions were set at 333 nm （Em） and 460 nm （Ex） using fluorescence detector （FLD）.Result： the linear detection ranges of OTA was 1.00 ~20.00 ng/mL with correlation coefficients（R2） of 0.998. Recovery rates in wheat spiked with OTA were in the range of 82.9 %~90.1 %,with the relative standard deviation of 5.1%~6.1%.The whole analytical was 72.8% and 87.5% lower than the national standard.Condusion： this method is suitable for determination of Ochratoxin A in wheat and is sensitively,efficiently and environment-friendly.It can save a lot of time and material in bulk sample analysis.

关 键 词：小麦 赭曲霉毒素A 超高效液相色谱 免疫亲和柱 漩涡提取 

分 类 号：S512.1[农业科学—作物学]