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固相萃取-高效液相色谱串联质谱法检测粮食中赭曲霉毒素A 预览 被引量:3

Application of solid-phase extraction to determination of ochratoxin A in grains by high performance liquid chromatography-tandem mass spec-trometry
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摘要 为了测定多种粮食样品中的赭曲霉毒素A(Ochratoxins A,OTA),建立了一种固相萃取-高效液相色谱串联质谱的检测方法。小麦、玉米、大豆和大米样品经乙腈-水(体积比80∶20)提取后,采用氨基固相萃取柱进行富集和洗脱,高效液相色谱串联质谱法进行检测。结果表明,不同粮食中赭曲霉毒素A在0.5-10.0μg/kg线性关系良好,相关系数(r)为0.999,定量限和检出限分别为0.50μg/kg和0.25μg/kg,日内和日间精密度的相对标准偏差(RSD)分别为1.71%-3.53%和0.69%-1.58%,重复性的相对标准偏差为3.72%-5.56%,加标回收率为83.2%-98.6%,相对标准偏差为2.26%-6.25%。 In order to determine the ochratoxin A ( OTA) in different grains,a method was developed for the deter-mination of OTA in wheat, corn, soybean,and rice by solid-phase extraction ( SPE) -high performance liquid chromatogra-phy-tandem mass spectrometry ( LC-MS/MS). After extracted by acetonitrile-water (80 :2 0,V /V ) and purified with NH2 -SPE column,OTA was detected by HPLC-MS/MS. The results showed that the linear correlation coefficient (r) was greater than 0. 999 in the range of 0. 5-10. 0 μg/kg. The limits of quantitation ( LOQ) and detection ( LOD) were 0.50 μg/kg and 0. 25 μg /k g ,and the relative standard deviation ( RSD) of repeatability was ranged from 3. 72% to 5. 56%. The RSD of in-tra-day and inter-day precision were ranged from 1. 71 % to 3. 53% and 0. 69% to 1. 58% , respectively. At different spiked levels , the recover ies were ranged f rom 83. 2% to 98. 6 % , and the RSD wasranged from 2.26% to 6. 25% .
作者 孙月 赵晋铭 贾雯晴 田中伟 董飞 SUN Yue 1, ZHAO Jin -mi ng 2, JIA Wen -qi ng 3, TI AN Zhong -wei4 , DONG Fe i5(1. Key Laboratory of National Meat Quality and Safety Control Engineering Research Center,Nanjing Agricultural University,Nanjing 210095,China; 2. National Center of Soybean Improvement/State Key Laboratory of Crop Genetics and Germplasm Enhancement/ College of Agriculture,Nanjing Agricultur-al University,Nanjing 210095, China; 3. The Academy of Science,Nanjing Agricultural University,Nanjing 210095, China; 4. Agronomy College of Nanjing Agricultural University/Key Laboratory of Crop Physiology Ecology and Production Management of Ministry of Agriculture,Nanjing 210095,Chi-na ;5. Institute of Food Quality and Safety,Jiangsu Academy of Agricultural Sciences,Nanjing 210014,China)
出处 《江苏农业学报》 CSCD 北大核心 2016年第6期1416-1420,共5页 Jiangsu Journal of Agricultural Sciences
基金 中央高校基本科研业务费专项资金项目(KJQN201632、KJSY201618)
关键词 固相萃取 高效液相色谱串联质谱法 赭曲霉毒素A 粮食 sol id-phase extraction HPLC -MS / MS ochratoxin A grain
作者简介 孙月(1989-),女,安徽蚌埠人,硕士研究生,主要从事农产品质量安全分析检测研究.(Tel)010-59199383;(E-mail)sunyuenjau@163.com
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