农产品中黄曲霉毒素B_1、B_2、G_1、G_2的超高效液相色谱-质谱联用检测分析

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目的应用超高效液相色谱-质谱联用(UPLC-MS/MS)技术,建立农产品中黄曲霉毒素B_1、B_2、G_1、G_2的定量检测方法,并对市场中的农产品进行检测分析。方法样品粉碎后,经乙腈-水(84∶16,V/V)提取,不经免疫亲和柱净化,氮吹浓缩定容后过0.22μm滤膜。滤液经Agilent Poroshell120ec-C_(18)反向色谱柱分离,以0.1%甲酸水-甲醇作为流动相梯度洗脱分离4种黄曲霉毒素。质谱采用电喷雾离子化源(ESI),正离子模式扫描。结果 4种黄曲霉毒素在各自的定量范围内均呈良好的线性关系(r>0.990),检出限为0.015μg/kg~0.095μg/kg(S/N=3),方法回收率为85.0%~90.6%,相对标准偏差为0.29%~7.20%。结论该方法简化了前处理操作,具有简便、快速、经济、灵敏、准确等优点,适用于多种农产品中黄曲霉毒素的检测。 OBJECTIVE To establish a quantitative method for the determination of aflatoxins B_1, B_2, G_1, G_2 in agricultural products by UPLC-MS / MS and to detect and analyze the agricultural products in the market. Methods After the sample was crushed, it was extracted with acetonitrile-water (84:16, V / V) and purified by immunoaffinity column. The filtrate was concentrated by nitrogen and filtered through a 0.22 μm filter. The filtrate was separated on an Agilent Poroshell 120ec-C 18 reversed-phase column and the four aflatoxins were eluted with a gradient elution of 0.1% formic acid in water-methanol. Mass spectrometry was performed using electrospray ionization source (ESI), positive ion mode. Results The four aflatoxins showed good linearity (r> 0.990) within the limits of quantification. The detection limits were 0.015μg / kg ~ 0.095μg / kg (S / N = 3) % ~ 90.6%, the relative standard deviation of 0.29% ~ 7.20%. Conclusion This method is simple, rapid, economical, sensitive and accurate. It is suitable for the determination of aflatoxins in a variety of agricultural products.
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