建立了腰果中4种黄曲霉毒素的高教液相色谱-串联质谱检测方法(HPLC-MS/MS).样品用甲醇-水(8:2,v/v)溶液提取后用弗罗里硅土柱净化,5 mL丙酮-水-甲酸溶液(96:3.5:0.5,v/v/v)洗脱,氮吹至干,1 mL甲醇定容;在资生堂MG C18色谱柱(100mmx3.0mm,3μm)上梯度洗脱分离,然后采用电喷雾离子化三重四极杆串联质谱测定.实验结果表明,4种黄曲霉毒素在各自的线性范围内峰面积与其质量浓度线性关系良好,相关系数(r2)大于0.997;检出限(信噪比为3)为0.009~0.04μg/kg,定量限(信噪比为10)为0.03~0.12μg/kg;平均回收率为63.0%~78.5%,相对标准偏差为28%~91%,均符合痕量分析的要求.评价了基质效应,信号抑制/增强值为88.8%~99.4%,说明净化后的基质效应较小.该方法简单快速、准确可靠,可用于腰果中黄曲霉毒素的检测.
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