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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
引用本文:张秀尧,蔡欣欣,李毅.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[J].分析化学,2012,40(8):1267-1273.
作者姓名:张秀尧  蔡欣欣  李毅
作者单位:温州市疾病预防控制中心,温州,325001
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.

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

Rapid Quantification of Cereulide, Emetic Toxin of Bacillus Cereus, in Foods by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry
ZHANG Xiu-Yao , CAI Xin-Xin , LI Yi.Rapid Quantification of Cereulide, Emetic Toxin of Bacillus Cereus, in Foods by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2012,40(8):1267-1273.
Authors:ZHANG Xiu-Yao  CAI Xin-Xin  LI Yi
Institution:(Wenzhou Center for Disease Control and Prevention,Wenzhou 325001,China)
Abstract: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.
Keywords:Ultra performance liquid chromatography-tandem mass spectrometry  Bacillus cereus Cereulide  Emetic toxin  Food
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