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建立了山银花药材中黄曲霉毒素等4种真菌毒素的超高效液相色谱-串联质谱(UHPLC-MS/MS)分析方法,并对4种黄曲霉毒素的裂解规律进行了分析了讨论。样品加60%乙腈超声提取,加0.2 g N-丙基乙二胺(PSA)净化,氮气吹至近干并复溶。色谱条件为:Agilent SB C18色谱柱(50 mm×2.1 mm,i.d.1.8μm);流动相为在电喷雾电离源(ESI)正模式下采用多反应监测模式(MRM)进行测定,定量方法采用内标法。并对4个化合物的主要质谱碎片进行研究和分析。4种真菌毒素在各自线性范围内线性关系良好,r2不低于0.9964,空白样品的加标回收率为78.3%~92.5%。相对标准偏差为3.3%~7.7%,方法可用于山银花药材中黄曲霉毒素的检测。
A method for the determination of four mycotoxins, such as aflatoxins, was established by UHPLC-MS / MS. The cleavage patterns of four aflatoxins were also discussed. The sample was sonicated with 60% acetonitrile, and purified with 0.2 g N-propyl ethylenediamine (PSA). The chromatographic conditions were: Agilent SB C18 column (50 mm × 2.1 mm, id 1.8 μm); the mobile phase was determined by multi-reaction monitoring mode (MRM) in electrospray ionization source (ESI) positive mode, Standard method. The main mass spectrum fragments of 4 compounds were studied and analyzed. The four mycotoxins had good linearity in their respective linear ranges with r2 of not less than 0.9964 and spiked recoveries of 78.3% to 92.5% for blank samples. The relative standard deviations were 3.3% ~ 7.7%. The method can be used for the determination of aflatoxins in Shannxihua medicinal materials.