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目的建立测定枸杞果酒中赭曲霉毒素A(OTA)的高效液相色谱-串联质谱法。方法样品用免疫亲和柱净化,以Agilent Zorbax SB-C18色谱柱(2.1 mm×50 mm,3.5μm)分离;梯度洗脱流动相:水(含0.1%甲酸)和乙腈(含0.1%甲酸);流速:0.4 mL/min;进样量:10μL;电喷雾正离子多反应监测扫描模式(MRM)检测。结果该方法的定量限为0.02 ng/mL,在0.02～20 ng/mL内线性关系良好,加样水平分别为0.2、2、20 ng/mL时,其回收率分别为71.0%、83.7%、86.0%,相对标准偏差(RSD)分别为8.0%、9.0%、6.1%;在随机购买的12份市售枸杞果酒中测得OTA的含量为0.03～0.18 ng/mL,检出率为50.0%。结论赭曲霉毒素A在样品中的测定结果均低于欧盟限量;该方法简便、灵敏、准确,可应用于枸杞果酒中赭曲霉毒素A的测定。
Objective To establish a high performance liquid chromatography tandem mass spectrometry method for the determination of ochratoxin A (OTA) in wolfberry fruit wine. Methods The samples were separated on an Agilent Zorbax SB-C18 column (2.1 mm × 50 mm, 3.5 μm) using an immunoaffinity column. The gradient elution mobile phase consisted of water (containing 0.1% formic acid) and acetonitrile (containing 0.1% formic acid) ; Flow rate: 0.4 mL / min; injection volume: 10 μL; electrospray positive ion multiple reaction monitoring scan mode (MRM). Results The limit of quantification was 0.02 ng / mL and the linearity was within 0.02 ~ 20 ng / mL. The recoveries were 71.0% and 83.7% at the loading levels of 0.2, 2 and 20 ng / mL, respectively. The relative standard deviations (RSDs) were 8.0%, 9.0% and 6.1%, respectively. The OTA content was 0.03-0.18 ng / mL in 12 randomly purchased medlar wines with the detection rate of 50.0% . Conclusion The results of the determination of ochratoxin A in the samples are lower than the EU limit. The method is simple, sensitive and accurate and can be applied to the determination of ochratoxin A in wolfberry fruit wine.