摘要
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.
出处
《分析化学》
SCIE
CAS
CSCD
北大核心
2012年第8期1267-1273,共7页
Chinese Journal of Analytical Chemistry
关键词
超高效液相色谱串联质谱
蜡样芽孢杆菌
呕吐毒素
食品
Ultra performance liquid chromatography-tandem mass spectrometry； Bacillus cereus Cereulide； Emetic toxin； Food
