超高效液相色谱-串联质谱法同时测定番茄酱中18种真菌毒素

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~20.99);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。

Simultaneous determination of 18 kinds of mycotoxins in tomato paste by ultra performance liquid chromatography-tandem mass spectrometry

Objective To establish a rapid and accurate method for simultaneous determination of 18 kinds of mycotoxins in tomato paste by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 80% acetonitrile solution, cleaned up on a homemade SPE column and blown to nearly dry by nitrogen, separated by an Acquity CORTECS UPLC C18 column with a mixture of 1 mmol/L ammonium acetate and methanol as mobile phase for gradient elution. The mass spectrometry was operated in electrospray ionization+, electrospray ionization- modes and multiple reaction monitoring mode. The samples were quantified with the external matrix matched standard calibration. Results The proposed method showed good linear relationships with the correlation coefficients above 0.99. The recoveries spiked at 3 levels were ranged from 77.1% to 105.4% with RSDs of 0.48%~6.98%. Based on the experiment, a total of 35 samples of tomato paste were positive in 40 samples, and 6 kinds of fungus toxin were checked out. Conclusion The method is sensitive, simple, rapid, reliable, and repeatable, which can meet the requirements for detection of 18 kinds of mycotoxins in tomato paste.