超高效液相色谱串联质谱法检测食品中蜡样芽孢杆菌呕吐毒素Cereulide

Rapid Quantification of Cereulide,Emetic Toxin of Bacillus Cereus,in Foods by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

建立了快速检测食品中蜡样芽孢杆菌呕吐毒素Cereulide的超高效液相色谱三重四极杆质谱联用分析方法。样品提取液经硅胶和Carb固相萃取柱净化后,以0.1%甲酸-0.2 mmol/L乙酸铵溶液和0.1%甲酸-乙腈溶液作为流动相进行梯度洗脱,在Acquity BEH 300 C18柱上实现分离,正离子ESI-MS/MS MRM方式检测,以13C6-Cereulide作为内标的稳定同位素稀释法进行定量分析。一次进样分析时间为7 min。米饭、添加33%玉米胚油的米饭和婴儿配方奶粉中平均加标回收率分别为85.7%～87.5%,85.3%～110%和94.2%～113%;相对标准偏差为4.6%～13%,5.9%～9.1%和3.4%～6.5%(n=6);定量限为10 ng/kg(S/N=10)。方法灵敏、准确,适合于食品样品中Cereulide的测定,并已成功应用于食物中毒样品的检测。

A rapid UPLC-MS/MS method is described for the quantification of Cereulide,the emetic toxin of Bacillus cereus in foods.After extraction the sample solution was cleaned-up by SiO2 and Carb SPE procedures,the analysis of Cereulide was performed on an Acquity BEH 300 C18 column using gradient elution with 0.1% formic acid in 0.2 mmol/L ammonium acetate and 0.1% formic acid in acetonitrile,and detected by the positive electrospray ionization-MS/MS method under MRM mode,and quantified by a stable isotope dilution method using the 13C6-Cereulide as the internal standard.The cycle time of each analysis was 7.0 min.The average recoveries were 85.7%-87.5%,85.3%-110% and 94.2%-113% for Cereulide in boiled rice,boiled rice supplemented with 33% maize oil and formula baby milk powder with RSDs of 4.6%-13%,5.9%-9.1% and 3.4%-6.5%（n=6）,respectively.The limits of quantitation（S/N=10） were 10 ng/kg.The method was sensitive and selective for the detection of Cereulide in food,and has been successfully applied to the measurement of Cereulide in the samples resulting in food poisoning.