摘要
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 develop a sensitive and accurate method of high performance liquid chromatography-tandem mass spectrometry for the quantification of ochratxoin A（OTA）in wolfberry fruit wine.Methods Samples were cleaned up by immunoaffinity column（IAC）and then separated on Agilent Zorbax SB-C18 column（2.1 mm×50 mm,3.5 μm）.Gradient mobile phase was prepared with water（containing 0.1% formic acid）and acetonitrile（containing 0.1% formic acid）.Flow rate was set to 0.4 mL/min and the injection volume was 10 μL.Liquid chromatography-electrospray ionization-MS/MS（LC-ESI-MS/MS）in multiple reaction monitoring（MRM）was operated under positive electrospray ionization mode.Results The limit of quantification（LOQ）of the method was 0.02 ng/mL.The calibration curves showed a good linearity in the range of 0.02-20 ng/mL.The spiked levels were set at 0.2,2,and 20 ng/mL with the average recoveries of 71.0%,83.7%,and 86.0% and the relative standard deviations（RSDs）of 8.0%,9.0%,and 6.1%,respectively.OTA concentrations in the 12 samples investigated were between 0.03 ng/mL and 0.18 ng/mL,and the detection rate was 50.0%.Conclusion OTA concentrations in the samples investigated were all below the maximum allowable limit established by the European Community.The method was proved to be simple,rapid,sensitive,and suitable for the quantification of OTA in wolfberry fruit wine.
出处
《中国公共卫生》
CAS
CSCD
北大核心
2012年第11期1520-1522,共3页
Chinese Journal of Public Health
基金
科技部重大新药创制专项(2009ZX09502-025)
国家中医药管理局2008年度中医药行业科研专项(200807042)
