【摘要】 应用高效液相色谱-电喷雾串联四极杆质谱联用系统(HPLC-MS/MS),在多反应离子检测方式(MRM)下,对花生中的黄曲霉毒素B1进行检测。对花生中黄曲霉毒素B1的提取、净化、液相分离及串联质谱等相关检测参数进行了优化研究。用V(甲醇)∶V(水)=6∶4提取,OASIS HLB SPE小柱净化,定容过滤。采用V(甲醇)∶V(水)(含体积分数0.1%甲酸)=7∶3为流动相,前级离子313.0,二级离子241.1、269.1,ESI正离子方式检测,在3.3 min出峰。结果表明,在ESI正离子模式下,黄曲霉毒素B1在其线性定量范围0.1~50μg/kg内,相关系数达到0.9999,检出限为0.03μg/kg,最低定量限为0.1μg/kg。低、中、高浓度添加回收率范围为93%~105%。更多还原

【Abstract】 An analytical method for the determination of aflatoxin B1 in peanuts by high performance liquid chromatography-tandem mass spectrometry has been developed.This article focused on the optimization of extraction,clean-up,HPLC separation and MS/MS parameters of the analyte.Aflatoxin B1 was extracted by 60%(V/V) of methanol aqueous solution,and then it was purified by OASIS HLB SPE column.The eluted extract was analyzed by HPLC-MS/MS in positive ion mode using multiple reaction monitoring with a triple-quadruple mass spectrometer using an electrospray ionization source.An isocratic mobile phase composed of methanolwater(70/30)(V/V) was used,water with 0.1% formic acid(V/V).With the precursor ion =313.0 and the product ion =241.1、 269.1,the retention time of aflatoxin B1 was 3.30 min.Under the ESI+ analysis,a high correlation coefficients(>0.999) of aflatoxin B1 was obtained within linear range(0.1～50 μg/kg).Sample recoveries at three spiking levels ranged from 93% to 105%(relative standard deviation(RSD≤5%).Determination limit(S/N=3) was 0.03 μg/kg and quantification limit(S/N=10) was 0.1 μg/kg.更多还原