高效液相色谱-串联质谱法检测花生中的黄曲霉毒素B1

Determination of aflatoxin B_1 in peanuts by liquid chromatography-tandem mass spectrometry

应用高效液相色谱一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。用矿（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3．3min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，捡出限为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％。

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 isocratie mobile phase composed of methanol-water （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 ariatoxin 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.