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目的首次建立同时对腐乳中的6种黄曲霉毒素进行定性和定量分析的超高效液相色谱三重四极杆质谱确证方法。方法样品用84/16的乙腈/水混合匀桨超声提取3 min,上清液过免疫亲和柱净化富集,经过Agilent ZORBAX SB C-18色谱柱分离,以乙腈和10 mmol乙酸铵溶液为流动相,梯度洗脱,进行UHPLC/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。结果标准曲线的线性范围分别是:AFT B1:0.1μg/kg~10.0μg/kg,AFT B2:0.1μg/kg~20.0μg/kg,AFT G1:1.0μg/kg~10μg/kg,AFT G2:1.0μg/kg~10.0μg/kg,AFT M1:0.1μg/kg~10.0μg/kg,AFT M2:1.0μg/kg~10.0μg/kg。6种黄曲霉毒素的加样平均回收率为:80.1%~85.3%,相对标准偏差为2.3%~9.5%。结论本实验方法专属性强,灵敏度高,操作简单,快捷,可做腐乳中黄曲霉毒素(B1、B2、G1、G2、M1、M2)的检测方法。
OBJECTIVE To establish a method for the simultaneous determination of six aflatoxins in preserved bean curd by using triple quadrupole mass spectrometry (UPLC-MS). Methods The samples were homogenized with 84/16 acetonitrile / water and homogenized for 3 min. The supernatants were purified by immunoaffinity column and separated by Agilent ZORBAX SB C-18 column. Acetonitrile and 10 mmol ammonium acetate solution Mobile phase, gradient elution, UHPLC / 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 standard curve was: AFT B1: 0.1 μg / kg to 10.0 μg / kg, AFT B2: 0.1 μg / kg to 20.0 μg / kg, AFT G1: 1.0 μg / kg to 10.0 μg / kg, AFT M1: 0.1 μg / kg to 10.0 μg / kg, and AFT M2: 1.0 μg / kg to 10.0 μg / kg. The average recoveries of six aflatoxins were 80.1% ~ 85.3% with relative standard deviations of 2.3% ~ 9.5%. Conclusion The method is specific, sensitive and easy to operate. It can be used to detect aflatoxins (B1, B2, G1, G2, M1, M2) in bean curd.