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《化学分析计量》 2020年第06期
DOI:10.3969/j.issn.1008-6145.2020.06.003
分散固相萃取-超高效液相色谱-串联质谱法同时测定玉米油中4种黄曲霉毒素
李莉,李硕
中国食品药品检定研究院,北京 100050 
Simultaneous determination of 4 kinds of aflatoxins in corn oil by dispersive solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry
LI Li, LI Shuo
National Institutes for Food and Drug Control, Beijing 100050, China 
摘要:建立分散固相萃取-超高效液相色谱-串联质谱法同时测定玉米油中黄曲霉毒素B1,B2,G1,G2的方法。样品经乙腈水溶液振荡提取,然后盐析进行液体分配,通过DisQuE净化管(分散固相萃取)净化,以C18色谱柱进行分离,多反应监测模式检测,采用基质匹配标准曲线法定量分析。4种黄曲霉毒素的质量浓度在0.5~50 μg/L范围内与色谱峰面积呈良好的线性关系,相关系数均大于0.999,检出限和定量限分别为0.2 μg/kg和0.6 μg/kg。在3个加标浓度水平下,黄曲霉毒素B1,B2,G1,G2的平均加标回收率为81.3%~113.5%,测定结果的相对标准偏差为1.6%~9.6%(n=6)。该方法操作简便,检测成本低,定量准确,适于玉米油中黄曲霉毒素的快速测定。  
Abstract:Abstract A method for simultaneous determination of aflatoxin B1, B2, G1, G2 in corn oil by dispersive solid phase extraction with ultra performance liquid chromatography-tandem mass spectrometry was established. The samples were extracted with acetonitrile aqueous solution. The extracts of samples were purified with DisQuE clean-up tube(dispersive solid phase extraction) after liquid-liquid partition using salts. Aflatoxins were separated by C18 chromatography column and detected by multiple reaction monitoring mode. The matrix matching standard curve method was used for quantitative analysis. The mass concentration of four kinds of aflatoxins had a good linear relationship with the chromatographic peak area in the ranges of 0.5-50 μg/L, the correlation coefficients were all more than 0.999, the detection limit and quantitative limit were 0.2 μg/kg and 0.6 μg/kg, respectively. The average recoveries of aflatoxins at three spiked concentration levels were 81.3%-113.5%, and the relative standard deviations were1.6%-9.6%(n=6). This method is simple, cost-effective and quantitatively accurate, which is suitable for the rapid determination of aflatoxins in corn oil.  
关键词:分散固相萃取;超高效液相色谱-串联质谱法;玉米油;黄曲霉毒素 
Keywords:DisQuE; ultra performance liquid chromatography-tandem mass spectrometry; corn oil; aflatoxin 
基金:国家重点研发计划项目(2017YFC1601103) 
本文引用格式:
引用格式 李莉,李硕.分散固相萃取-超高效液相色谱-串联质谱法同时测定玉米油中4种黄曲霉毒素[J].化学分析计量,2020,29(6):10-14.
LI L,LI S. Simultaneous determination of 4 kinds of aflatoxins in corn oil by dispersive solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage,2020,29(6):10-14. 

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