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目的建立同时检测番茄酱中18种真菌毒素的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)分析方法。方法样品经80%乙腈溶液提取后,通过自制固相萃取柱排除杂质干扰,流出液经氮吹至近干后,采用Acquity CORTECS UPLC C_(18)色谱柱分离,用1mmol/L乙酸铵-甲醇作为流动相进行梯度洗脱,电喷雾正负离子模式电离,多反应监测模式检测,基质校准外标法定量。结果 18种毒素在各自浓度范围内呈现良好线性关系(r~2>0.99);在3个不同添加水平下的平均加标回收率均在77.1%~105.4%之间,相对标准偏差为0.48%~6.98%。利用本实验建立的方法对40份番茄酱样品进行检测,共有35份番茄酱样品呈阳性,检出6种真菌毒素。结论该方法灵敏度高,操作简单,快速可靠,重复性好,可满足对番茄酱中18种真菌毒素检测的要求。
Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) method for the simultaneous determination of 18 mycotoxins in tomato paste. Methods After the sample was extracted with 80% acetonitrile, impurities were eliminated by self-made solid-phase extraction (SPE) column. The effluent was blown to near dryness by nitrogen and was separated on an Acquity CORTECS UPLC C 18 column with 1 mmol / L ammonium acetate- Mobile phase gradient elution, electrospray positive and negative ionization mode, multi-reaction monitoring mode detection, matrix calibration external standard method. Results 18 kinds of toxins showed a good linear relationship (r ~ 2> 0.99) in the range of their respective concentrations. The average recoveries of spiked toxins at 77% to 105.4% and the relative standard deviations were 0.48% ~ 6.98%. Using the method established in this experiment, 40 samples of tomato sauce were tested. A total of 35 samples of tomato paste were positive, and 6 kinds of mycotoxins were detected. Conclusion The method has high sensitivity, simple operation, fast and reliable, good repeatability and can meet the requirements of 18 mycotoxins detection in tomato sauce.