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% .
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)