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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。
In this study, by optimizing the conditions of liquid chromatography and mass spectrometry conditions, combined with sodium bicarbonate solution extraction and dilution method effectively overcome the matrix effect interference, established in Chinese herbal medicine ochratoxin A by ultra performance liquid chromatography - tandem mass spectrometry method Check method. The sample was extracted by sodium bicarbonate solution, extracted by ultrasonic wave, purified by immunoaffinity column and separated by C18 liquid chromatography column. The multistage reaction was detected by ion-positive ion mode. The method validation showed that there was a good linear relationship between the concentration of ochratoxin A and the concentration of 0.1 ~ 50.0μg / L, r> 0.99. The recoveries of the samples at three spiked levels of 1.0, 2.0 and 10.0μg / kg were 78.5 % ~ 98.0%; the relative standard deviation was 2.6% ~ 11.8%; the detection limit was 1.0μg / kg. The method was applied to the actual detection of eight batches of samples, the results showed that one batch of eight batches of samples detected in the first batch of ochratoxin A test results were positive (7.3μg / kg). The actual sample test results show that this method can be used in Chinese herbal medicine Ochratoxin A sensitive and accurate qualitative and quantitative analysis.