摘要
研究优化了应用液相色谱-电喷雾串联四级杆质谱仪,用多离子反应监测定量法同时检测青贮玉米中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、呕吐毒素、玉米赤霉烯酮、麦角醇、杂色曲霉毒素、HT-2毒素和T-2毒素的方法。样品经乙腈-水-甲酸（8415.90.1,V/V）提取后,经Mycospin 400多功能净化柱净化后过膜直接上机测定,在5-100 ng/ml的线性范围内,线性关系良好。选择高中低3个浓度水平进行空白样品加标,平均回收率为67.4%-114.1%,相对标准偏差（RSD）为0.2%-6.1%,该方法精密度良好,回收率高,灵敏度好,在较短时间内同时能满足10种霉菌毒素的检测。利用该方法检测了2015年度4省市10个奶牛场的14个全株青贮玉米样品,其中河南3个,河北4个,黑龙江3个,山东4个。结果发现,10个奶牛场全株青贮玉米样品中全部检出的霉菌毒素种类为呕吐毒素、黄曲霉毒素B2和玉米赤霉烯酮,河南、河北和山东还检出麦角醇。奶牛场全株玉米青贮玉米样品中霉菌毒素含量由高到低依次为呕吐毒素、玉米赤霉烯酮、黄曲霉毒素B2和麦角醇,样品含量全部未超过国家限量。
This study optimized LC-MS/MS detection method to simultaneously test of aflatoxin B 1 （AFB1）, aflatoxin B2 （AFB2）, aflatoxin G1 （AFG1）, aflatoxin G2 （AFG2）, deoxynivalenol （DON）, zeara- lenone （ZEN）, lysergol, sterigmatocystin, HT-2 toxin and T-2 toxin in corn silage using multiple reac- tion monitoring （MRM） quantitative model. The sample was extracted using acetonitrile - water - after acid （84 ： 15.9 ： 0.1, V/V） and Myeospin 400 multifunction purified column, then detected by LC-MS/ MS. The average recovery was 67.4%-114.1%, and the relative standard deviation was 0.2%-6.1%.The mycotoxins of 14 corn silage samples from Henan, Hebei, Heilongjiang and Shandong were tested using this method. The results showed that deoxynivalenol, aflatoxin B2 and zearale- none were all detected, and shoud be concerned in corn silage, but the content of them does not exceed national limits.
出处
《饲料工业》
北大核心
2016年第19期45-49,共5页
Feed Industry
基金
农业技术试验示范专项经费
现代农业产业技术体系专项资金[nycytx-04-01]
公益性行业(农业)科研专项项目“生鲜乳质量安全评价技术与生产规程”[201403071]
中国农业科学院科技创新工程[ASTIP-IAS12]
