超高效液相色谱-串联质谱法检测中草药中赭曲霉毒素A  

Determination of Ochratoxin A in Chinese Medicinal Plants by UHPLC-MS/MS

作　　者：薛良辰[1] 刘陆[1] 郑璇[2] 姚丽锋[1] 冯家望[1] 蔡勤仁[1] 

机构地区：[1]珠海出入境检验检疫局,广东珠海519015 [2]广东出入境检验检疫局,广东广州510623

出　　处：《现代食品科技》2016年第10期297-303,316,共8页Modern Food Science and Technology

基　　金：2014年珠海市本级农业专项资金项目(2014ZH26)

摘　　要：本研究通过优化液相色谱条件和质谱条件,并结合碳酸氢钠溶液提取稀释的方法法有效克服了基质效应的干扰,建立了中草药中赭曲霉毒素A的超高效液相色谱-串联质谱法快速检方法。试样经碳酸氢钠溶液提取,超声波提取,再经过免疫亲和柱净化后,用C18液相色谱柱分离,多级反应选择离子正离子模式检测。经方法学验证,赭曲霉毒素A质量浓度在0.1-50.0μg/L范围内呈现良好的线性关系,r〉0.99;样品在1.0、2.0和10.0μg/kg三个添加水平下的回收率为78.5%-98.0%;相对标准偏差为2.6%-11.8%;方法检出限为1.0μg/kg。将该方法应用于实际8批样品的检测,结果显示8批样品中检出1批的赭曲霉毒素A检测结果呈阳性（7.3μg/kg）。实际样品检测结果表明,本方法可实现中草药中赭曲霉毒素A灵敏、准确的定性定量分析。A rapid method for the determination of ochratoxin A in Chinese medicinal plants using ultra-high performance liquid chromatography tandem mass spectrometry （UHPLC-MS/MS） was established in this study. For this method, the conditions required for liquid chromatography （LC） and mass spectrometry （MS） were optimized and the matrix effects were overcome by extraction using sodium bicarbonate solution and dilution procedure. The ultrasonic-assisted extraction of ochratoxin A from the sample was carried out using sodium bicarbonate solution, followed by an immunoaffinity colunm clean-up procedure. The analytes were separated on a C18 LC column and detected on a mass spectrometer operating in the positive ion multiple reaction monitoring （MRM） mode. The method used in the present study was validated. Ochratoxin A concentration showed good linearity in the range of 0.1-50.0μg/L, with an r-value〉0.99. The average recoveries ranged between 78.5% and 98.0% at spike levels of 1.0, 2.0, and 10.0 μg/kg. The relative standard deviations （RSDs） were between 2.6% and 11.8%, and the limit of detection was 1.0 μg/kg. The validated method was applied for the detection of ochratoxin A in eight batches of samples, and the results showed one positive result per batch （7.3μg/kg）. The results of the real sample test indicate that this method can be used for the sensitive and accurate determination of ochratoxin A in Chinese medicinal plants.

关 键 词：赭曲霉毒素A 超高效液相色谱串联质谱 中草药 

分 类 号：R284.1[医药卫生—中药学] O657.63[医药卫生—中医学]