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目的:通过优化液相色谱条件和质谱条件,并结合稀释法克服基质效应的影响,建立适用于10种中药材和3种食品污染赭曲霉毒素A(OTA)的LC-MS/MS检测方法。方法:样品经84%乙腈提取后,上清液用色谱甲醇复溶(稀释4倍),直接上样检测;流动相采用4.0 mmol·L-1醋酸铵-0.1%甲酸水溶液和甲醇,经C18色谱柱分离后注入质谱仪,在选择反应监测模式(SRM)下进行正离子检测。结果:经方法学验证,赭曲霉毒素A质量浓度在25.00~50 000 ng·L-1范围内呈现良好的线性关系,r>0.998 7;定量限25.0 ng·L-1;高、中、低3个浓度水平的绝对回收率89.6%~95.2%,提取回收率84.2%~100.0%;13种样品的基质效应91.5%~118.7%。将该方法应用于实际100批样品的检测,结果显示100批样品中仅有1批的检测结果呈阳性(0.7μg·kg-1),表明该地区这些样品中OTA的污染情况不严重。结论:本研究建立的LC-MS/MS方法具有预处理简便、经济等优点,适用于这10种中药材及3种食品污染赭曲霉毒素A的快速检测。
OBJECTIVE: To establish an LC-MS / MS method for the determination of ochratoxin A (OTA), which is suitable for 10 kinds of traditional Chinese medicines and 3 kinds of foodstuffs, by optimizing the conditions of liquid chromatography and mass spectrometry and combing the influence of matrix effect by dilution method. Methods: After the sample was extracted with 84% acetonitrile, the supernatant was re-dissolved by chromatography (diluted 4-fold) and directly tested. The mobile phase was treated with 4.0 mmol·L -1 ammonium acetate-0.1% formic acid in water and methanol, The column is separated and injected into the mass spectrometer for positive ion detection in a selective reaction monitoring mode (SRM). Results: The method validation showed that the ochratoxin A concentration in the range of 25.00 ~ 50 000 ng · L-1 showed a good linear relationship, r> 0.998 7; the limit of quantification was 25.0 ng · L-1; The absolute recoveries of three concentration levels ranged from 89.6% to 95.2% and the recoveries ranged from 84.2% to 100.0%. The matrix effects of the 13 samples ranged from 91.5% to 118.7%. The method was applied to the actual detection of 100 batches of samples. The results showed that only one of the 100 batches of samples showed positive results (0.7 μg · kg -1), indicating that the OTA pollution in these samples was not serious. Conclusion: The LC-MS / MS method established in this study has the advantages of simple and economical pretreatment, and is suitable for the rapid detection of ochratoxin A in these 10 kinds of Chinese herbal medicines and 3 kinds of foodstuffs.