石墨化碳黑净化—超高效液相色谱法快速检测食品中黄曲霉毒素B_(1)

Rapid determination of aflatoxin B_(1) in food by GCB purification and ultra-high performance liquid chromatography

建立了一种使用石墨化碳黑(GCB)净化、超高效液相色谱大体积流通池快速检测食品中黄曲霉毒素B1的方法。5 g样品中加入20 mL甲醇-水(体积比8∶2)溶液振荡均匀并离心。取10 mL上清液于另一离心管中,加入石墨化碳黑(花生油0.06 g,稻谷、玉米、花生各0.1 g),振荡离心去除上清液;沉淀加入8 mL甲醇振荡离心去除上清液。沉淀于110℃放置15 min后加入0.2 g无水硫酸镁,分2次每次加入5 mL二硫化碳涡旋振荡,离心合并2次上清液于40℃水浴中氮气吹干;以1 mL初始流动相复溶,超高效液相色谱仪分析。在此条件下,样品检出限为0.02μg/kg,标准曲线相关系数为0.9999,加标样回收率为88.9%~97.5%,RSD 2.9%~5.9%(N=6)。方法符合国家标准要求,操作简单,提高了样品检测效率,降低了检测成本。

A method for rapid detection of aflatoxin B_(1) in food using graphitized carbon black(GCB)purification and ultra-high performance liquid chromatography large-volume flow cell was established.Add 20 mL of methanol-water(volume ratio 8∶2)solution was added to 5 g sample,and then was uniformly vibrated and centrifuged.10 mL of the supernatant was taken into another centrifuge tube and graphitized carbon black(0.06 g of peanut oil,0.1 g of rice,corn,peanut)was added,then supernatant was removed by centrifuge;The precipitate was added with 8 mL methanoland supernatant was removed by centrifugation.The precipitate was placed at 110℃for 15 minutes,0.2 g anhydrous magnesium sulfate was added,then 5 mL carbon disulfide was added in two separate times for vortexandcentrifuge.Two supernatants were combined and dried in a water bath at 40℃and blow dry with nitrogen.Resolution with 1 mL of initial mobile phase andanalyzed by ultra-high performance liquid chromatography.Under these conditions,the detection limit of the sample was 0.02μg/kg,the correlation coefficient of the standard curve was 0.9999,the recovery rate of standard addition were 88.9%~97.5%,RSD 2.9%~5.9%(N=6).The methed accords with the national standard and is easy to operate,which inproves the efficiency of sample detection and reduces the cost.