【摘要】 建立了超声提取-液相色谱-电喷雾三重串联四极杆质谱测定玉米、大米、大豆等粮油固体样品中黄曲霉毒素B1、B2、G1和G2(AFB1、AFB2、AFG1和AFG2)的方法。分析前对样品进行超声提取,优化得到最佳超声提取条件:溶剂为甲醇-水(含40 g/L NaCl)(80∶20,v/v)溶液、料液比为1∶3(g∶mL)、温度为50℃、时间为3 min。然后对提取的样品进行免疫亲和特异性净化。最后与液相色谱-电喷雾三重串联四极杆质谱联用,使用C18反相色谱柱,流动相为甲醇-10 mmol/L乙酸铵水溶液梯度洗脱,以黄曲霉毒素M1(AFM1)作为内标进行定量测定。结果表明,AFB1、AFB2、AFG1和AFG2的检出限分别为0.002、0.004、0.004和0.012μg/kg。方法的加标回收率为87%～111%,日内相对标准偏差(RSD)和日间RSD分别不大于6.7%和5.6%。实验结果表明该方法可以有效地降低基质效应的影响,相比于外标法能极大地提高方法的准确度。更多还原

【Abstract】 The high performance liquid chromatography(HPLC)-triple quadrupole tandem mass spectrometry was applied for the determination of the aflatoxins: B1(AFB1),B2(AFB2),G1(AFG1) and G2(AFG2),in cereals and oils.The samples were first extracted by ultrasonic method.The optimized conditions of ultrasonic extraction were as follows: temperature of 50 ℃,extraction time of 3 min, methanol-water(containing 40 g/L NaCl)(80∶20,v/v) solution as the medium and a ratio of sample to solvent of 1∶3(g∶mL).The extracts were then purified using an immunoaffinity column.The separation was performed on a C18 column with mobile phases of 10 mmol/L ammonium acetate and methanol in gradient elution.The sensitive detection of the four AFT compounds by electrospray ionization mass spectrometry(ESI-MS) was carried out in selected reaction monitoring(SRM) mode with aflatoxin M1(AFM1) as the internal standard.Under the optimized conditions,the limits of detection of AFB1,AFB2,AFG1 and AFG2 were 0.002,0.004,0.004 and 0.012 μg/kg,respectively.The recoveries of aflatoxins in different spiked cereals and oils were in the range from 87% to 111%.The intraday and inter-day precisions were not more than 6.7% and 5.6%,respectively.In comparison with the external standard method,this method can effectively inhibit the matrix effects,and greatly improve the accuracy.更多还原