摘要
建立了免疫亲和柱净化/超高效液相色谱法快速测定粮食中呕吐毒素(DON)的检测方法。样品经纯水提取后,用免疫亲和柱净化、浓缩,Waters Acquity UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱分离,以甲醇-水(10∶90)为流动相,流速为0.1 mL/min,进样量1μL,用Acquity紫外检测器在220 nm处进行检测,保留体积不足0.5 mL,整个分析过程用时不足45 min。呕吐毒素在0.5～10.0 mg/L范围内线性关系良好,相关系数(r2)为0.999 96;检出限(S/N=3)为0.15 ng,定量下限(S/N=10)为0.5 ng,加标回收率为84%～98%,相对标准偏差为2.9%～5.9%。该方法简便快速、灵敏度高、重现性好、溶剂用量少且环保,适用于原粮中呕吐毒素的快速测定。
A rapid and environmental-friendly analytic method was established for the determination of deoxynivalenol（DON） in grain samples. The samples were extracted with water, cleaned up with immunoaffinity column（IAC）. The separation of targeted compound was performed on a Waters Acquity UPLC BEH C18 （2-1 mm × 50 mm, 1.7 μm） using methanolwater（ 10 ： 90） as mobile phase with a flow rate of 0. 1 mL/min at 25 ℃. The injection volume was 1 μL for UV detection at 220 nm and the retention volume was less than 0. 5 mL. The whole process from sample pretreatment to analysis took less than 45 min. The linear range of deoxynivalenol was in the range of 0. 5 - 10. 0 mg/L with a correlation coefficient of 0.999 96. The limit of detection（LOD） was 0. 15 ng and the limit of quantitation（LOQ） was 0.5 ng. The average recoveries were between 84% and 98% with RSDs of 2. 9% - 5.9% . The method was suitable for the determination of DON in the raw grain, with advantages of simplicity, rapidness, sensitivity, good reproducibility and environment friendly.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第12期1362-1366,共5页
Journal of Instrumental Analysis
基金
国家十一五科技支撑计划(2006BAD08B07-2)
