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目的建立UPLC-MS/MS检测腐乳中4种黄曲霉毒素的方法。方法样品用乙腈/水(86/14,V/V)混合匀浆超声提取10 min,高速离心,上清液过多功能净化柱MycosepTM226,氮气吹至近干,初始流动相定容,0.22μm微孔滤膜过滤,经过Agilent ZORBAX XDB C18色谱柱分离,以乙腈和0.1%甲酸溶液为流动相,梯度洗脱,进行UPLC-MS/MS分析。质谱采用正离子扫描模式,离子源为ESI(+),定量检测方式为多反应监测(MRM)方式,利用保留时间和碎片信号比值判定定性结果。结果方法的线性范围为0.001μg/kg~0.16μg/kg,线性相关系数均>0.999 0,检出限为0.001μg/kg~0.009μg/kg;低、中、高3个水平的平均加标回收率为96.4%~99.7%,相对标准偏差(RSD)均<2.0%。结论该方法用于测定腐乳中4种黄曲霉毒素具有操作简单、干扰少、快速、准确可靠等特点,可作为腐乳中黄曲霉毒素检测的确证方法。为市场监督提供良好的基础数据。
Objective To establish a UPLC-MS / MS method for the determination of four aflatoxins in bean curd. Methods The samples were extracted with acetonitrile / water (86/14, V / V) for 10 min. The supernatant was centrifuged at high speed. MycosepTM226 was purged with supernatant. The nitrogen was blown to near dryness and the initial mobile phase consisted of 0.22 μm micro The membrane was filtered through a filter and separated on an Agilent ZORBAX XDB C18 column using a mobile phase of acetonitrile and 0.1% formic acid as the mobile phase, gradient elution and UPLC-MS / MS analysis. The mass spectrometry was carried out in positive ion scan mode with ESI (+) ion source and multiple reaction monitoring (MRM) as quantitative detection method. The qualitative results were judged by the retention time and fragment signal ratio. Results The linear range of the method was 0.001μg / kg ~ 0.16μg / kg, the linear correlation coefficient was> 0.999 0, the detection limit was 0.001μg / kg ~ 0.009μg / kg; The recoveries ranged from 96.4% to 99.7% with relative standard deviations (RSDs) <2.0%. Conclusion The method was applied to the determination of four aflatoxins in bean curd with simple operation, less interference, fast, accurate and reliable. It can be used as a confirmatory method for aflatoxins in preserved bean curd. Provide good basic data for market supervision.